# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Gregory Solan' _publ_contact_author_email GAS8@LE.AC.UK _publ_section_title ; Bis(imino)quaterpyridine-bearing multimetallic late transition metal complexes as ethylene oligomerisation catalysts ; loop_ _publ_author_name 'Gregory Solan' 'Yohan D M Champouret' 'Qudsia Khamker' 'Kuldip Singh' # Attachment '08086 rev.cif' data_08086 _database_code_depnum_ccdc_archive 'CCDC 733356' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C56 H67 Cl3 Co4 N14)(Co Cl4)24(C H3 C N)' _chemical_formula_sum 'C160 H206 Cl10 Co5 N38' _chemical_formula_weight 3310.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.280(5) _cell_length_b 31.251(9) _cell_length_c 16.942(5) _cell_angle_alpha 90.00 _cell_angle_beta 116.399(6) _cell_angle_gamma 90.00 _cell_volume 7721(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 783 _cell_measurement_theta_min 2.403 _cell_measurement_theta_max 27.066 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3474 _exptl_absorpt_coefficient_mu 0.765 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7809 _exptl_absorpt_correction_T_max 0.9071 _exptl_absorpt_process_details ; absorption correction based on 6201 reflections(SADABS);Rint 0.1148 before correction and 0.0652 after. ; _exptl_special_details ; The data was weak due to crystal quality. Efforts to refine the CoCl4 unit with full occupancy gave oversized ellipsoids. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59445 _diffrn_reflns_av_R_equivalents 0.1860 _diffrn_reflns_av_sigmaI/netI 0.2769 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15166 _reflns_number_gt 5136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Disordered CH3CN was omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 2430.5 \%A3 with an estimated 1134e/cell to be added.Forty eight solvent CH3CN molecules/unit cell accounting for 1056e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst.A46, C-34. The isopropyl carbon atoms are disordered and attempts to split these atoms failed .The data was weak and C55 could not be refined as a "decent" ellipsoid Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1031P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15166 _refine_ls_number_parameters 673 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2110 _refine_ls_R_factor_gt 0.0933 _refine_ls_wR_factor_ref 0.2462 _refine_ls_wR_factor_gt 0.2139 _refine_ls_goodness_of_fit_ref 0.834 _refine_ls_restrained_S_all 0.834 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.27243(7) 0.56458(3) 0.39193(7) 0.0321(3) Uani 1 1 d . . . Co2 Co 0.18758(7) 0.56934(4) 0.57382(7) 0.0400(3) Uani 1 1 d . . . Cl1 Cl 0.28787(14) 0.51134(6) 0.30174(13) 0.0424(5) Uani 1 1 d . . . Cl2 Cl 0.24977(14) 0.60956(6) 0.50274(13) 0.0436(6) Uani 1 1 d . . . Cl3 Cl 0.25932(14) 0.52330(7) 0.68495(13) 0.0483(6) Uani 1 1 d . . . N1 N 0.2919(5) 0.6257(2) 0.3324(4) 0.0397(17) Uani 1 1 d . . . N2 N 0.4054(4) 0.57970(18) 0.4641(4) 0.0299(15) Uani 1 1 d . . . N3 N 0.3215(4) 0.51794(18) 0.4986(4) 0.0326(15) Uani 1 1 d . . . N4 N 0.1304(4) 0.5189(2) 0.4700(4) 0.0400(17) Uani 1 1 d . . . N5 N 0.0546(4) 0.5839(2) 0.5093(4) 0.0433(19) Uani 1 1 d . . . N6 N 0.1752(5) 0.6274(2) 0.6451(4) 0.0414(18) Uani 1 1 d . . . N7 N 0.1365(6) 0.5655(2) 0.3138(5) 0.054(2) Uani 1 1 d . . . C1 C 0.2191(6) 0.6440(3) 0.2524(5) 0.042(2) Uani 1 1 d . . . C2 C 0.2054(6) 0.6298(2) 0.1684(5) 0.039(2) Uani 1 1 d . . . C3 C 0.1315(6) 0.6454(3) 0.0956(5) 0.048(2) Uani 1 1 d . . . H3 H 0.1198 0.6347 0.0391 0.057 Uiso 1 1 calc R . . C4 C 0.0740(6) 0.6760(3) 0.1018(5) 0.047(2) Uani 1 1 d . . . C5 C 0.0894(6) 0.6897(2) 0.1822(6) 0.046(2) Uani 1 1 d . . . H5 H 0.0483 0.7103 0.1857 0.056 Uiso 1 1 calc R . . C6 C 0.1612(5) 0.6760(2) 0.2611(5) 0.038(2) Uani 1 1 d . . . C7 C 0.2686(6) 0.5980(3) 0.1588(5) 0.055(3) Uani 1 1 d . . . H7 H 0.3049 0.5848 0.2180 0.066 Uiso 1 1 calc R . . C8 C 0.3371(7) 0.6201(3) 0.1321(6) 0.081(3) Uani 1 1 d . . . H8A H 0.3040 0.6321 0.0728 0.121 Uiso 1 1 calc R . . H8B H 0.3820 0.5991 0.1326 0.121 Uiso 1 1 calc R . . H8C H 0.3688 0.6431 0.1740 0.121 Uiso 1 1 calc R . . C9 C 0.2142(8) 0.5613(3) 0.0941(6) 0.095(4) Uani 1 1 d . . . H9A H 0.1682 0.5497 0.1109 0.142 Uiso 1 1 calc R . . H9B H 0.2567 0.5384 0.0969 0.142 Uiso 1 1 calc R . . H9C H 0.1835 0.5725 0.0339 0.142 Uiso 1 1 calc R . . C10 C 0.1758(5) 0.6935(2) 0.3506(5) 0.038(2) Uani 1 1 d . . . H10 H 0.2311 0.6795 0.3978 0.045 Uiso 1 1 calc R . . C11 C 0.0904(6) 0.6845(3) 0.3687(6) 0.056(3) Uani 1 1 d . . . H11A H 0.0342 0.6930 0.3173 0.084 Uiso 1 1 calc R . . H11B H 0.0964 0.7009 0.4203 0.084 Uiso 1 1 calc R . . H11C H 0.0876 0.6539 0.3799 0.084 Uiso 1 1 calc R . . C12 C 0.1922(6) 0.7422(3) 0.3530(5) 0.061(3) Uani 1 1 d . . . H12A H 0.2382 0.7483 0.3319 0.091 Uiso 1 1 calc R . . H12B H 0.2142 0.7526 0.4135 0.091 Uiso 1 1 calc R . . H12C H 0.1347 0.7567 0.3149 0.091 Uiso 1 1 calc R . . C13 C -0.0077(6) 0.6920(3) 0.0200(6) 0.067(3) Uani 1 1 d . . . H13 H -0.0295 0.7180 0.0396 0.081 Uiso 1 1 calc R . . C14 C -0.0893(8) 0.6608(4) -0.0134(8) 0.162(8) Uani 1 1 d . . . H14A H -0.0768 0.6368 -0.0435 0.244 Uiso 1 1 calc R . . H14B H -0.1449 0.6757 -0.0546 0.244 Uiso 1 1 calc R . . H14C H -0.0982 0.6502 0.0367 0.244 Uiso 1 1 calc R . . C15 C 0.0199(8) 0.7083(4) -0.0512(7) 0.110(4) Uani 1 1 d . . . H15A H 0.0615 0.7328 -0.0281 0.165 Uiso 1 1 calc R . . H15B H -0.0352 0.7172 -0.1036 0.165 Uiso 1 1 calc R . . H15C H 0.0508 0.6854 -0.0670 0.165 Uiso 1 1 calc R . . C16 C 0.4004(5) 0.6832(3) 0.3479(5) 0.053(2) Uani 1 1 d . . . H16A H 0.3497 0.6943 0.2943 0.079 Uiso 1 1 calc R . . H16B H 0.4543 0.6788 0.3373 0.079 Uiso 1 1 calc R . . H16C H 0.4152 0.7037 0.3961 0.079 Uiso 1 1 calc R . . C17 C 0.3731(6) 0.6417(3) 0.3724(6) 0.042(2) Uani 1 1 d . . . C18 C 0.4389(6) 0.6177(3) 0.4478(5) 0.043(2) Uani 1 1 d . . . C19 C 0.5254(6) 0.6318(3) 0.4991(6) 0.049(2) Uani 1 1 d . . . H19 H 0.5465 0.6580 0.4860 0.059 Uiso 1 1 calc R . . C20 C 0.5831(6) 0.6072(3) 0.5716(5) 0.046(2) Uani 1 1 d . . . H20 H 0.6444 0.6159 0.6077 0.055 Uiso 1 1 calc R . . C21 C 0.5475(6) 0.5685(3) 0.5903(5) 0.043(2) Uani 1 1 d . . . H21 H 0.5832 0.5515 0.6404 0.052 Uiso 1 1 calc R . . C22 C 0.4599(5) 0.5572(2) 0.5328(5) 0.0226(17) Uani 1 1 d . . . C23 C 0.4146(5) 0.5188(2) 0.5473(5) 0.0263(17) Uani 1 1 d . . . C24 C 0.4632(5) 0.4861(2) 0.6051(5) 0.036(2) Uani 1 1 d . . . H24 H 0.5276 0.4883 0.6398 0.043 Uiso 1 1 calc R . . C25 C 0.4160(5) 0.4505(2) 0.6111(5) 0.036(2) Uani 1 1 d . . . H25 H 0.4475 0.4272 0.6483 0.043 Uiso 1 1 calc R . . C26 C 0.3215(6) 0.4496(2) 0.5615(5) 0.036(2) Uani 1 1 d . . . H26 H 0.2876 0.4253 0.5635 0.044 Uiso 1 1 calc R . . C27 C 0.2761(6) 0.4845(2) 0.5087(5) 0.0341(19) Uani 1 1 d . . . C28 C 0.1737(6) 0.4837(3) 0.4583(5) 0.041(2) Uani 1 1 d . . . C29 C 0.1269(6) 0.4520(3) 0.4008(6) 0.058(3) Uani 1 1 d . . . H29 H 0.1586 0.4279 0.3938 0.070 Uiso 1 1 calc R . . C30 C 0.0323(7) 0.4552(3) 0.3525(6) 0.062(3) Uani 1 1 d . . . H30 H -0.0011 0.4335 0.3113 0.075 Uiso 1 1 calc R . . C31 C -0.0123(6) 0.4898(3) 0.3648(5) 0.054(3) Uani 1 1 d . . . H31 H -0.0770 0.4923 0.3328 0.065 Uiso 1 1 calc R . . C32 C 0.0380(6) 0.5211(3) 0.4241(5) 0.050(3) Uani 1 1 d . . . C33 C -0.0049(6) 0.5622(3) 0.4415(6) 0.050(2) Uani 1 1 d . . . C34 C -0.0935(6) 0.5739(3) 0.3872(6) 0.060(3) Uani 1 1 d . . . H34 H -0.1318 0.5561 0.3394 0.072 Uiso 1 1 calc R . . C35 C -0.1248(7) 0.6107(4) 0.4028(7) 0.079(4) Uani 1 1 d . . . H35 H -0.1856 0.6201 0.3665 0.095 Uiso 1 1 calc R . . C36 C -0.0639(7) 0.6353(4) 0.4756(7) 0.070(3) Uani 1 1 d . . . H36 H -0.0849 0.6614 0.4888 0.084 Uiso 1 1 calc R . . C37 C 0.0267(6) 0.6221(3) 0.5287(6) 0.050(3) Uani 1 1 d . . . C38 C 0.0962(6) 0.6449(3) 0.6079(5) 0.045(2) Uani 1 1 d . . . C39 C 0.0686(6) 0.6861(3) 0.6362(6) 0.071(3) Uani 1 1 d . . . H39A H 0.1150 0.6940 0.6953 0.106 Uiso 1 1 calc R . . H39B H 0.0092 0.6822 0.6371 0.106 Uiso 1 1 calc R . . H39C H 0.0635 0.7089 0.5946 0.106 Uiso 1 1 calc R . . C40 C 0.2449(6) 0.6437(3) 0.7203(6) 0.052(2) Uani 1 1 d . . . C41 C 0.3042(6) 0.6773(3) 0.7180(6) 0.051(2) Uani 1 1 d . . . C42 C 0.3769(6) 0.6900(3) 0.7961(6) 0.056(3) Uani 1 1 d . . . H42 H 0.4178 0.7109 0.7933 0.067 Uiso 1 1 calc R . . C43 C 0.3937(7) 0.6739(4) 0.8785(7) 0.068(3) Uani 1 1 d . . . C44 C 0.3374(7) 0.6423(4) 0.8808(7) 0.072(3) Uani 1 1 d . . . H44 H 0.3498 0.6295 0.9359 0.086 Uiso 1 1 calc R . . C45 C 0.2602(7) 0.6276(3) 0.8035(6) 0.068(3) Uani 1 1 d . . . C46 C 0.2899(6) 0.6976(3) 0.6304(5) 0.052(2) Uani 1 1 d . . . H46 H 0.2371 0.6835 0.5807 0.063 Uiso 1 1 calc R . . C47 C 0.2695(7) 0.7465(3) 0.6320(6) 0.070(3) Uani 1 1 d . . . H47A H 0.2200 0.7503 0.6493 0.104 Uiso 1 1 calc R . . H47B H 0.2509 0.7587 0.5732 0.104 Uiso 1 1 calc R . . H47C H 0.3248 0.7611 0.6744 0.104 Uiso 1 1 calc R . . C48 C 0.3758(7) 0.6941(3) 0.6154(6) 0.072(3) Uani 1 1 d . . . H48A H 0.4263 0.7099 0.6617 0.108 Uiso 1 1 calc R . . H48B H 0.3631 0.7062 0.5577 0.108 Uiso 1 1 calc R . . H48C H 0.3930 0.6639 0.6173 0.108 Uiso 1 1 calc R . . C49 C 0.4796(7) 0.6873(4) 0.9622(6) 0.082(3) Uani 1 1 d . . . H49 H 0.5055 0.7140 0.9495 0.098 Uiso 1 1 calc R . . C50 C 0.5539(9) 0.6538(5) 0.9982(10) 0.231(11) Uani 1 1 d . . . H50A H 0.5775 0.6521 1.0623 0.346 Uiso 1 1 calc R . . H50B H 0.6039 0.6615 0.9835 0.346 Uiso 1 1 calc R . . H50C H 0.5286 0.6260 0.9720 0.346 Uiso 1 1 calc R . . C51 C 0.4590(9) 0.6951(5) 1.0362(7) 0.155(7) Uani 1 1 d . . . H51A H 0.4292 0.6698 1.0461 0.232 Uiso 1 1 calc R . . H51B H 0.4179 0.7198 1.0231 0.232 Uiso 1 1 calc R . . H51C H 0.5160 0.7009 1.0892 0.232 Uiso 1 1 calc R . . C52 C 0.1951(6) 0.5932(3) 0.8126(6) 0.061(3) Uani 1 1 d . . . H52 H 0.1596 0.5794 0.7537 0.073 Uiso 1 1 calc R . . C53 C 0.2497(8) 0.5574(3) 0.8805(6) 0.100(4) Uani 1 1 d . . . H53A H 0.2710 0.5684 0.9405 0.150 Uiso 1 1 calc R . . H53B H 0.3025 0.5486 0.8712 0.150 Uiso 1 1 calc R . . H53C H 0.2096 0.5326 0.8722 0.150 Uiso 1 1 calc R . . C54 C 0.1286(6) 0.6167(3) 0.8364(6) 0.074(3) Uani 1 1 d . . . H54A H 0.1625 0.6356 0.8867 0.111 Uiso 1 1 calc R . . H54B H 0.0929 0.5961 0.8521 0.111 Uiso 1 1 calc R . . H54C H 0.0870 0.6339 0.7860 0.111 Uiso 1 1 calc R . . C55 C 0.0661(10) 0.5696(3) 0.2550(9) 0.088(4) Uani 1 1 d . . . C56 C -0.0302(8) 0.5745(5) 0.1678(9) 0.194(9) Uani 1 1 d . . . H56A H -0.0228 0.5946 0.1270 0.291 Uiso 1 1 calc R . . H56B H -0.0769 0.5853 0.1842 0.291 Uiso 1 1 calc R . . H56C H -0.0492 0.5466 0.1391 0.291 Uiso 1 1 calc R . . Co3 Co 0.72656(15) 0.69292(6) 0.47285(17) 0.0474(6) Uani 0.50 1 d P . . Cl4 Cl 0.6416(3) 0.65382(12) 0.3446(3) 0.0500(12) Uani 0.50 1 d P . . Cl5 Cl 0.8309(3) 0.73252(14) 0.4456(4) 0.0728(16) Uani 0.50 1 d P . . Cl6 Cl 0.8062(3) 0.65343(13) 0.5943(3) 0.0556(13) Uani 0.50 1 d P . . Cl7 Cl 0.6320(3) 0.73590(13) 0.4999(4) 0.0731(17) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0454(7) 0.0232(6) 0.0365(6) 0.0074(5) 0.0261(6) 0.0078(5) Co2 0.0484(8) 0.0466(8) 0.0337(7) 0.0074(6) 0.0260(6) 0.0128(6) Cl1 0.0555(14) 0.0308(11) 0.0410(12) 0.0002(9) 0.0216(11) 0.0091(10) Cl2 0.0659(16) 0.0355(11) 0.0450(13) 0.0010(9) 0.0386(13) 0.0103(10) Cl3 0.0582(15) 0.0553(15) 0.0335(12) 0.0118(10) 0.0223(11) 0.0176(11) N1 0.058(5) 0.031(4) 0.037(4) 0.007(3) 0.027(4) 0.013(4) N2 0.048(4) 0.021(3) 0.028(4) 0.008(3) 0.024(3) 0.008(3) N3 0.040(4) 0.022(4) 0.046(4) -0.003(3) 0.028(4) -0.004(3) N4 0.037(4) 0.059(5) 0.032(4) 0.017(3) 0.022(4) 0.003(4) N5 0.036(4) 0.072(6) 0.032(4) 0.011(4) 0.024(4) 0.010(4) N6 0.048(5) 0.053(5) 0.028(4) 0.009(3) 0.021(4) 0.017(4) N7 0.071(6) 0.033(4) 0.066(6) -0.005(4) 0.039(5) 0.003(5) C1 0.063(6) 0.036(5) 0.044(6) 0.003(4) 0.038(5) -0.001(4) C2 0.066(6) 0.022(4) 0.039(5) 0.000(4) 0.034(5) 0.002(4) C3 0.076(7) 0.040(6) 0.029(5) 0.001(4) 0.025(5) -0.006(5) C4 0.066(6) 0.038(5) 0.023(5) 0.003(4) 0.008(5) -0.016(5) C5 0.066(6) 0.018(4) 0.052(6) 0.009(4) 0.023(5) -0.004(4) C6 0.054(6) 0.020(4) 0.046(5) 0.006(4) 0.028(5) -0.003(4) C7 0.096(8) 0.042(6) 0.035(5) 0.007(4) 0.035(6) 0.016(5) C8 0.120(9) 0.082(8) 0.070(7) -0.008(6) 0.069(7) 0.014(7) C9 0.203(13) 0.035(6) 0.075(8) -0.013(5) 0.087(9) 0.012(7) C10 0.056(6) 0.024(4) 0.040(5) 0.010(4) 0.027(5) 0.015(4) C11 0.080(7) 0.030(5) 0.058(6) -0.002(4) 0.031(6) 0.006(5) C12 0.096(8) 0.036(6) 0.047(6) -0.018(4) 0.029(6) -0.006(5) C13 0.086(8) 0.036(6) 0.036(6) 0.014(4) -0.012(5) -0.005(5) C14 0.149(12) 0.098(11) 0.102(10) 0.057(8) -0.070(9) -0.064(9) C15 0.125(11) 0.117(11) 0.086(9) 0.048(8) 0.046(8) 0.054(8) C16 0.060(6) 0.049(6) 0.044(6) 0.023(4) 0.018(5) -0.001(5) C17 0.047(6) 0.040(5) 0.055(6) 0.008(4) 0.038(5) 0.000(4) C18 0.050(6) 0.039(5) 0.042(5) -0.002(4) 0.023(5) 0.009(5) C19 0.051(6) 0.041(6) 0.052(6) 0.005(5) 0.021(5) -0.003(5) C20 0.053(6) 0.039(5) 0.040(5) -0.002(4) 0.016(5) -0.001(4) C21 0.057(6) 0.032(5) 0.036(5) 0.009(4) 0.017(5) 0.013(4) C22 0.034(5) 0.017(4) 0.023(4) -0.001(3) 0.019(4) -0.001(3) C23 0.035(5) 0.024(4) 0.027(4) 0.000(3) 0.021(4) 0.005(4) C24 0.046(5) 0.033(5) 0.044(5) 0.011(4) 0.033(4) 0.010(4) C25 0.044(6) 0.021(4) 0.043(5) 0.005(4) 0.019(5) 0.007(4) C26 0.056(6) 0.028(5) 0.041(5) -0.001(4) 0.036(5) -0.007(4) C27 0.053(5) 0.024(4) 0.042(5) 0.009(4) 0.036(4) 0.016(4) C28 0.036(6) 0.056(6) 0.036(5) 0.018(5) 0.021(4) 0.010(5) C29 0.048(6) 0.066(7) 0.058(7) -0.023(5) 0.021(5) -0.032(5) C30 0.065(7) 0.080(8) 0.054(7) -0.021(6) 0.038(6) -0.019(6) C31 0.027(5) 0.097(8) 0.029(5) -0.009(5) 0.005(4) -0.012(5) C32 0.024(5) 0.094(8) 0.025(5) 0.009(5) 0.004(4) -0.005(5) C33 0.037(6) 0.078(7) 0.042(6) 0.012(5) 0.023(5) 0.011(5) C34 0.035(6) 0.106(9) 0.040(6) -0.004(6) 0.018(5) 0.023(6) C35 0.035(6) 0.136(12) 0.059(7) 0.027(7) 0.014(6) 0.027(7) C36 0.064(7) 0.106(9) 0.059(7) 0.038(7) 0.046(6) 0.047(7) C37 0.058(6) 0.064(7) 0.048(6) 0.022(5) 0.041(5) 0.038(5) C38 0.043(6) 0.056(6) 0.033(5) 0.014(4) 0.015(5) 0.025(5) C39 0.098(8) 0.050(7) 0.083(8) -0.008(5) 0.058(7) 0.022(6) C40 0.067(7) 0.063(7) 0.032(6) 0.016(5) 0.026(5) 0.011(5) C41 0.056(6) 0.054(6) 0.036(6) 0.010(5) 0.015(5) 0.034(5) C42 0.048(6) 0.069(7) 0.047(6) 0.000(5) 0.019(5) 0.022(5) C43 0.061(8) 0.099(9) 0.049(7) -0.008(6) 0.029(6) 0.028(6) C44 0.080(8) 0.098(10) 0.053(7) -0.006(6) 0.043(7) 0.015(7) C45 0.083(8) 0.082(8) 0.034(6) -0.004(5) 0.022(6) 0.033(6) C46 0.078(7) 0.057(6) 0.036(5) -0.004(4) 0.038(5) 0.009(5) C47 0.100(8) 0.064(7) 0.045(6) 0.001(5) 0.032(6) 0.024(6) C48 0.102(8) 0.060(7) 0.066(7) -0.002(5) 0.049(7) 0.005(6) C49 0.090(9) 0.110(10) 0.047(7) -0.008(6) 0.032(7) 0.026(7) C50 0.103(12) 0.220(19) 0.208(17) -0.126(14) -0.077(11) 0.106(12) C51 0.179(14) 0.239(18) 0.072(9) -0.104(10) 0.080(10) -0.077(13) C52 0.091(8) 0.056(7) 0.069(7) 0.015(5) 0.066(6) 0.005(6) C53 0.197(13) 0.053(7) 0.071(7) 0.016(6) 0.079(9) 0.044(8) C54 0.102(8) 0.086(8) 0.060(7) 0.006(6) 0.060(7) 0.013(6) C55 0.129(12) 0.043(7) 0.142(13) 0.015(8) 0.104(10) -0.030(8) C56 0.058(9) 0.28(2) 0.160(15) 0.108(14) -0.031(9) -0.059(11) Co3 0.0403(13) 0.0198(12) 0.0916(19) -0.0031(12) 0.0380(13) -0.0026(11) Cl4 0.056(3) 0.018(2) 0.093(4) 0.014(2) 0.048(3) 0.0001(19) Cl5 0.055(3) 0.030(3) 0.147(5) 0.001(3) 0.057(3) -0.001(2) Cl6 0.068(3) 0.025(2) 0.101(4) 0.006(2) 0.061(3) 0.009(2) Cl7 0.052(3) 0.021(2) 0.151(5) -0.001(3) 0.049(3) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N7 2.011(8) . ? Co1 N2 2.013(6) . ? Co1 N3 2.179(6) . ? Co1 N1 2.248(6) . ? Co1 Cl1 2.347(2) . ? Co1 Cl2 2.501(2) . ? Co2 N5 1.996(7) . ? Co2 N4 2.233(7) . ? Co2 N6 2.239(7) . ? Co2 Cl3 2.241(2) . ? Co2 Cl2 2.267(2) . ? N1 C17 1.289(9) . ? N1 C1 1.463(9) . ? N2 C22 1.311(8) . ? N2 C18 1.386(9) . ? N3 C27 1.334(8) . ? N3 C23 1.366(8) . ? N4 C32 1.354(9) . ? N4 C28 1.368(10) . ? N5 C33 1.315(10) . ? N5 C37 1.370(10) . ? N6 C38 1.276(9) . ? N6 C40 1.372(10) . ? N7 C55 1.144(13) . ? C1 C2 1.412(10) . ? C1 C6 1.424(10) . ? C2 C3 1.373(10) . ? C2 C7 1.490(10) . ? C3 C4 1.376(11) . ? C3 H3 0.9500 . ? C4 C5 1.339(10) . ? C4 C13 1.517(11) . ? C5 C6 1.396(10) . ? C5 H5 0.9500 . ? C6 C10 1.528(10) . ? C7 C8 1.540(12) . ? C7 C9 1.563(11) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.544(10) . ? C10 C11 1.576(10) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.539(12) . ? C13 C15 1.548(13) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.486(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.458(11) . ? C18 C19 1.359(10) . ? C19 C20 1.398(10) . ? C19 H19 0.9500 . ? C20 C21 1.437(10) . ? C20 H20 0.9500 . ? C21 C22 1.369(9) . ? C21 H21 0.9500 . ? C22 C23 1.484(9) . ? C23 C24 1.392(9) . ? C24 C25 1.381(9) . ? C24 H24 0.9500 . ? C25 C26 1.388(9) . ? C25 H25 0.9500 . ? C26 C27 1.395(10) . ? C26 H26 0.9500 . ? C27 C28 1.498(10) . ? C28 C29 1.360(11) . ? C29 C30 1.389(11) . ? C29 H29 0.9500 . ? C30 C31 1.370(12) . ? C30 H30 0.9500 . ? C31 C32 1.379(11) . ? C31 H31 0.9500 . ? C32 C33 1.553(12) . ? C33 C34 1.372(10) . ? C34 C35 1.332(13) . ? C34 H34 0.9500 . ? C35 C36 1.417(13) . ? C35 H35 0.9500 . ? C36 C37 1.405(11) . ? C36 H36 0.9500 . ? C37 C38 1.496(12) . ? C38 C39 1.511(11) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C45 1.411(11) . ? C40 C41 1.441(12) . ? C41 C42 1.384(11) . ? C41 C46 1.533(11) . ? C42 C43 1.391(12) . ? C42 H42 0.9500 . ? C43 C44 1.360(13) . ? C43 C49 1.542(13) . ? C44 C45 1.428(12) . ? C44 H44 0.9500 . ? C45 C52 1.565(13) . ? C46 C48 1.532(11) . ? C46 C47 1.566(11) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C51 1.455(12) . ? C49 C50 1.509(14) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C54 1.506(11) . ? C52 C53 1.567(12) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.614(16) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? Co3 Cl7 2.239(5) . ? Co3 Cl6 2.251(5) . ? Co3 Cl5 2.308(5) . ? Co3 Cl4 2.335(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Co1 N2 165.5(3) . . ? N7 Co1 N3 116.5(3) . . ? N2 Co1 N3 75.8(2) . . ? N7 Co1 N1 91.5(3) . . ? N2 Co1 N1 75.2(2) . . ? N3 Co1 N1 150.2(3) . . ? N7 Co1 Cl1 89.2(2) . . ? N2 Co1 Cl1 99.43(17) . . ? N3 Co1 Cl1 87.72(16) . . ? N1 Co1 Cl1 103.49(16) . . ? N7 Co1 Cl2 90.0(2) . . ? N2 Co1 Cl2 83.70(17) . . ? N3 Co1 Cl2 82.83(16) . . ? N1 Co1 Cl2 87.48(16) . . ? Cl1 Co1 Cl2 169.01(8) . . ? N5 Co2 N4 76.1(3) . . ? N5 Co2 N6 77.0(3) . . ? N4 Co2 N6 153.0(3) . . ? N5 Co2 Cl3 129.79(19) . . ? N4 Co2 Cl3 95.02(18) . . ? N6 Co2 Cl3 101.87(18) . . ? N5 Co2 Cl2 102.35(19) . . ? N4 Co2 Cl2 95.80(16) . . ? N6 Co2 Cl2 90.32(17) . . ? Cl3 Co2 Cl2 127.82(9) . . ? Co2 Cl2 Co1 109.69(9) . . ? C17 N1 C1 123.6(7) . . ? C17 N1 Co1 114.3(5) . . ? C1 N1 Co1 122.0(5) . . ? C22 N2 C18 117.8(7) . . ? C22 N2 Co1 122.2(5) . . ? C18 N2 Co1 119.5(5) . . ? C27 N3 C23 117.9(6) . . ? C27 N3 Co1 127.6(5) . . ? C23 N3 Co1 112.7(4) . . ? C32 N4 C28 117.9(8) . . ? C32 N4 Co2 112.7(6) . . ? C28 N4 Co2 128.4(5) . . ? C33 N5 C37 117.8(8) . . ? C33 N5 Co2 124.0(6) . . ? C37 N5 Co2 117.6(6) . . ? C38 N6 C40 122.4(8) . . ? C38 N6 Co2 113.2(6) . . ? C40 N6 Co2 124.4(6) . . ? C55 N7 Co1 163.5(9) . . ? C2 C1 C6 120.7(8) . . ? C2 C1 N1 120.7(7) . . ? C6 C1 N1 118.6(7) . . ? C3 C2 C1 118.5(7) . . ? C3 C2 C7 120.7(7) . . ? C1 C2 C7 120.9(8) . . ? C2 C3 C4 122.1(8) . . ? C2 C3 H3 118.9 . . ? C4 C3 H3 118.9 . . ? C5 C4 C3 118.3(8) . . ? C5 C4 C13 121.1(9) . . ? C3 C4 C13 120.6(8) . . ? C4 C5 C6 125.1(8) . . ? C4 C5 H5 117.5 . . ? C6 C5 H5 117.5 . . ? C5 C6 C1 115.3(8) . . ? C5 C6 C10 122.4(7) . . ? C1 C6 C10 122.4(7) . . ? C2 C7 C8 111.0(7) . . ? C2 C7 C9 111.3(8) . . ? C8 C7 C9 112.4(7) . . ? C2 C7 H7 107.3 . . ? C8 C7 H7 107.3 . . ? C9 C7 H7 107.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C12 109.1(6) . . ? C6 C10 C11 111.6(7) . . ? C12 C10 C11 109.2(6) . . ? C6 C10 H10 109.0 . . ? C12 C10 H10 109.0 . . ? C11 C10 H10 109.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C4 C13 C14 112.9(7) . . ? C4 C13 C15 112.4(8) . . ? C14 C13 C15 115.1(9) . . ? C4 C13 H13 105.1 . . ? C14 C13 H13 105.1 . . ? C15 C13 H13 105.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C18 116.3(8) . . ? N1 C17 C16 123.8(8) . . ? C18 C17 C16 119.9(8) . . ? C19 C18 N2 122.6(8) . . ? C19 C18 C17 122.9(8) . . ? N2 C18 C17 114.5(7) . . ? C18 C19 C20 119.0(8) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C19 C20 C21 118.5(8) . . ? C19 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? C22 C21 C20 117.1(7) . . ? C22 C21 H21 121.4 . . ? C20 C21 H21 121.4 . . ? N2 C22 C21 124.9(7) . . ? N2 C22 C23 113.0(7) . . ? C21 C22 C23 121.9(7) . . ? N3 C23 C24 122.7(7) . . ? N3 C23 C22 114.6(6) . . ? C24 C23 C22 122.7(7) . . ? C25 C24 C23 118.9(8) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C24 C25 C26 118.3(7) . . ? C24 C25 H25 120.9 . . ? C26 C25 H25 120.9 . . ? C25 C26 C27 120.1(7) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? N3 C27 C26 121.9(8) . . ? N3 C27 C28 118.7(7) . . ? C26 C27 C28 119.4(7) . . ? C29 C28 N4 122.0(8) . . ? C29 C28 C27 123.2(8) . . ? N4 C28 C27 114.7(8) . . ? C28 C29 C30 119.4(9) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C31 C30 C29 119.4(9) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C32 119.1(9) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? N4 C32 C31 122.2(9) . . ? N4 C32 C33 114.2(8) . . ? C31 C32 C33 123.5(8) . . ? N5 C33 C34 126.5(9) . . ? N5 C33 C32 112.0(8) . . ? C34 C33 C32 121.4(9) . . ? C35 C34 C33 118.5(10) . . ? C35 C34 H34 120.7 . . ? C33 C34 H34 120.7 . . ? C34 C35 C36 117.4(9) . . ? C34 C35 H35 121.3 . . ? C36 C35 H35 121.3 . . ? C37 C36 C35 121.8(10) . . ? C37 C36 H36 119.1 . . ? C35 C36 H36 119.1 . . ? N5 C37 C36 117.9(9) . . ? N5 C37 C38 115.5(7) . . ? C36 C37 C38 126.5(9) . . ? N6 C38 C37 115.7(8) . . ? N6 C38 C39 125.9(8) . . ? C37 C38 C39 118.5(7) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N6 C40 C45 120.2(9) . . ? N6 C40 C41 122.1(8) . . ? C45 C40 C41 117.7(9) . . ? C42 C41 C40 118.7(8) . . ? C42 C41 C46 120.4(9) . . ? C40 C41 C46 120.9(8) . . ? C41 C42 C43 124.1(10) . . ? C41 C42 H42 118.0 . . ? C43 C42 H42 118.0 . . ? C44 C43 C42 117.2(10) . . ? C44 C43 C49 121.2(10) . . ? C42 C43 C49 121.2(11) . . ? C43 C44 C45 122.5(10) . . ? C43 C44 H44 118.8 . . ? C45 C44 H44 118.8 . . ? C40 C45 C44 119.6(10) . . ? C40 C45 C52 121.1(9) . . ? C44 C45 C52 119.3(9) . . ? C48 C46 C41 111.9(7) . . ? C48 C46 C47 106.8(8) . . ? C41 C46 C47 109.2(7) . . ? C48 C46 H46 109.6 . . ? C41 C46 H46 109.6 . . ? C47 C46 H46 109.6 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C51 C49 C50 102.6(12) . . ? C51 C49 C43 112.1(9) . . ? C50 C49 C43 114.8(10) . . ? C51 C49 H49 109.0 . . ? C50 C49 H49 109.0 . . ? C43 C49 H49 109.0 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C54 C52 C45 106.8(8) . . ? C54 C52 C53 113.2(7) . . ? C45 C52 C53 112.0(8) . . ? C54 C52 H52 108.2 . . ? C45 C52 H52 108.2 . . ? C53 C52 H52 108.2 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N7 C55 C56 176.1(13) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? Cl7 Co3 Cl6 108.1(2) . . ? Cl7 Co3 Cl5 110.72(18) . . ? Cl6 Co3 Cl5 107.51(19) . . ? Cl7 Co3 Cl4 109.10(19) . . ? Cl6 Co3 Cl4 115.20(17) . . ? Cl5 Co3 Cl4 106.2(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Co2 Cl2 Co1 -98.2(2) . . . . ? N4 Co2 Cl2 Co1 -21.23(19) . . . . ? N6 Co2 Cl2 Co1 -174.92(19) . . . . ? Cl3 Co2 Cl2 Co1 79.73(13) . . . . ? N7 Co1 Cl2 Co2 73.8(2) . . . . ? N2 Co1 Cl2 Co2 -119.34(18) . . . . ? N3 Co1 Cl2 Co2 -42.94(18) . . . . ? N1 Co1 Cl2 Co2 165.3(2) . . . . ? Cl1 Co1 Cl2 Co2 -12.1(5) . . . . ? N7 Co1 N1 C17 171.4(6) . . . . ? N2 Co1 N1 C17 -2.7(5) . . . . ? N3 Co1 N1 C17 10.6(8) . . . . ? Cl1 Co1 N1 C17 -99.1(5) . . . . ? Cl2 Co1 N1 C17 81.4(5) . . . . ? N7 Co1 N1 C1 -11.6(6) . . . . ? N2 Co1 N1 C1 174.3(6) . . . . ? N3 Co1 N1 C1 -172.4(5) . . . . ? Cl1 Co1 N1 C1 77.9(5) . . . . ? Cl2 Co1 N1 C1 -101.6(5) . . . . ? N7 Co1 N2 C22 152.1(10) . . . . ? N3 Co1 N2 C22 3.2(5) . . . . ? N1 Co1 N2 C22 176.4(6) . . . . ? Cl1 Co1 N2 C22 -82.0(5) . . . . ? Cl2 Co1 N2 C22 87.3(5) . . . . ? N7 Co1 N2 C18 -20.2(13) . . . . ? N3 Co1 N2 C18 -169.1(6) . . . . ? N1 Co1 N2 C18 4.1(5) . . . . ? Cl1 Co1 N2 C18 105.7(5) . . . . ? Cl2 Co1 N2 C18 -84.9(5) . . . . ? N7 Co1 N3 C27 14.3(7) . . . . ? N2 Co1 N3 C27 -174.0(6) . . . . ? N1 Co1 N3 C27 172.7(5) . . . . ? Cl1 Co1 N3 C27 -73.7(6) . . . . ? Cl2 Co1 N3 C27 100.7(6) . . . . ? N7 Co1 N3 C23 178.7(5) . . . . ? N2 Co1 N3 C23 -9.6(4) . . . . ? N1 Co1 N3 C23 -22.9(7) . . . . ? Cl1 Co1 N3 C23 90.7(4) . . . . ? Cl2 Co1 N3 C23 -94.9(4) . . . . ? N5 Co2 N4 C32 -6.0(5) . . . . ? N6 Co2 N4 C32 -5.1(8) . . . . ? Cl3 Co2 N4 C32 123.8(5) . . . . ? Cl2 Co2 N4 C32 -107.3(5) . . . . ? N5 Co2 N4 C28 -174.2(6) . . . . ? N6 Co2 N4 C28 -173.2(5) . . . . ? Cl3 Co2 N4 C28 -44.4(6) . . . . ? Cl2 Co2 N4 C28 84.5(6) . . . . ? N4 Co2 N5 C33 -0.7(6) . . . . ? N6 Co2 N5 C33 179.8(7) . . . . ? Cl3 Co2 N5 C33 -85.5(7) . . . . ? Cl2 Co2 N5 C33 92.3(6) . . . . ? N4 Co2 N5 C37 -171.0(6) . . . . ? N6 Co2 N5 C37 9.4(5) . . . . ? Cl3 Co2 N5 C37 104.1(6) . . . . ? Cl2 Co2 N5 C37 -78.1(5) . . . . ? N5 Co2 N6 C38 -7.1(5) . . . . ? N4 Co2 N6 C38 -8.0(9) . . . . ? Cl3 Co2 N6 C38 -135.6(5) . . . . ? Cl2 Co2 N6 C38 95.5(5) . . . . ? N5 Co2 N6 C40 174.0(7) . . . . ? N4 Co2 N6 C40 173.1(6) . . . . ? Cl3 Co2 N6 C40 45.5(6) . . . . ? Cl2 Co2 N6 C40 -83.4(6) . . . . ? N2 Co1 N7 C55 62(4) . . . . ? N3 Co1 N7 C55 -152(3) . . . . ? N1 Co1 N7 C55 38(3) . . . . ? Cl1 Co1 N7 C55 -65(3) . . . . ? Cl2 Co1 N7 C55 126(3) . . . . ? C17 N1 C1 C2 92.8(10) . . . . ? Co1 N1 C1 C2 -83.9(8) . . . . ? C17 N1 C1 C6 -88.4(9) . . . . ? Co1 N1 C1 C6 94.9(7) . . . . ? C6 C1 C2 C3 -4.1(12) . . . . ? N1 C1 C2 C3 174.7(7) . . . . ? C6 C1 C2 C7 176.9(7) . . . . ? N1 C1 C2 C7 -4.3(12) . . . . ? C1 C2 C3 C4 3.7(12) . . . . ? C7 C2 C3 C4 -177.3(8) . . . . ? C2 C3 C4 C5 -2.4(13) . . . . ? C2 C3 C4 C13 -179.2(8) . . . . ? C3 C4 C5 C6 1.6(13) . . . . ? C13 C4 C5 C6 178.4(8) . . . . ? C4 C5 C6 C1 -2.0(12) . . . . ? C4 C5 C6 C10 178.9(7) . . . . ? C2 C1 C6 C5 3.2(11) . . . . ? N1 C1 C6 C5 -175.6(7) . . . . ? C2 C1 C6 C10 -177.7(7) . . . . ? N1 C1 C6 C10 3.5(11) . . . . ? C3 C2 C7 C8 79.5(10) . . . . ? C1 C2 C7 C8 -101.5(9) . . . . ? C3 C2 C7 C9 -46.5(11) . . . . ? C1 C2 C7 C9 132.4(8) . . . . ? C5 C6 C10 C12 -60.6(10) . . . . ? C1 C6 C10 C12 120.4(8) . . . . ? C5 C6 C10 C11 60.1(9) . . . . ? C1 C6 C10 C11 -118.9(8) . . . . ? C5 C4 C13 C14 -98.4(11) . . . . ? C3 C4 C13 C14 78.3(13) . . . . ? C5 C4 C13 C15 129.3(10) . . . . ? C3 C4 C13 C15 -53.9(11) . . . . ? C1 N1 C17 C18 -176.0(7) . . . . ? Co1 N1 C17 C18 0.9(9) . . . . ? C1 N1 C17 C16 6.6(12) . . . . ? Co1 N1 C17 C16 -176.5(6) . . . . ? C22 N2 C18 C19 1.1(11) . . . . ? Co1 N2 C18 C19 173.7(6) . . . . ? C22 N2 C18 C17 -177.7(6) . . . . ? Co1 N2 C18 C17 -5.1(9) . . . . ? N1 C17 C18 C19 -176.4(7) . . . . ? C16 C17 C18 C19 1.1(12) . . . . ? N1 C17 C18 N2 2.4(10) . . . . ? C16 C17 C18 N2 179.9(7) . . . . ? N2 C18 C19 C20 -0.4(12) . . . . ? C17 C18 C19 C20 178.3(7) . . . . ? C18 C19 C20 C21 -1.7(12) . . . . ? C19 C20 C21 C22 3.0(11) . . . . ? C18 N2 C22 C21 0.4(10) . . . . ? Co1 N2 C22 C21 -172.0(5) . . . . ? C18 N2 C22 C23 175.8(6) . . . . ? Co1 N2 C22 C23 3.5(8) . . . . ? C20 C21 C22 N2 -2.4(11) . . . . ? C20 C21 C22 C23 -177.5(6) . . . . ? C27 N3 C23 C24 1.0(10) . . . . ? Co1 N3 C23 C24 -165.0(5) . . . . ? C27 N3 C23 C22 -179.6(6) . . . . ? Co1 N3 C23 C22 14.3(7) . . . . ? N2 C22 C23 N3 -12.1(8) . . . . ? C21 C22 C23 N3 163.5(6) . . . . ? N2 C22 C23 C24 167.2(6) . . . . ? C21 C22 C23 C24 -17.2(10) . . . . ? N3 C23 C24 C25 2.6(11) . . . . ? C22 C23 C24 C25 -176.6(6) . . . . ? C23 C24 C25 C26 -2.4(11) . . . . ? C24 C25 C26 C27 -1.3(10) . . . . ? C23 N3 C27 C26 -4.9(10) . . . . ? Co1 N3 C27 C26 158.7(5) . . . . ? C23 N3 C27 C28 177.9(6) . . . . ? Co1 N3 C27 C28 -18.5(9) . . . . ? C25 C26 C27 N3 5.2(11) . . . . ? C25 C26 C27 C28 -177.6(7) . . . . ? C32 N4 C28 C29 1.7(11) . . . . ? Co2 N4 C28 C29 169.4(6) . . . . ? C32 N4 C28 C27 177.8(6) . . . . ? Co2 N4 C28 C27 -14.6(9) . . . . ? N3 C27 C28 C29 121.4(9) . . . . ? C26 C27 C28 C29 -55.8(10) . . . . ? N3 C27 C28 N4 -54.5(9) . . . . ? C26 C27 C28 N4 128.2(7) . . . . ? N4 C28 C29 C30 -0.1(13) . . . . ? C27 C28 C29 C30 -175.8(7) . . . . ? C28 C29 C30 C31 -1.2(13) . . . . ? C29 C30 C31 C32 0.8(13) . . . . ? C28 N4 C32 C31 -2.1(11) . . . . ? Co2 N4 C32 C31 -171.6(6) . . . . ? C28 N4 C32 C33 -179.8(6) . . . . ? Co2 N4 C32 C33 10.7(8) . . . . ? C30 C31 C32 N4 0.8(13) . . . . ? C30 C31 C32 C33 178.4(8) . . . . ? C37 N5 C33 C34 0.1(12) . . . . ? Co2 N5 C33 C34 -170.3(6) . . . . ? C37 N5 C33 C32 176.7(7) . . . . ? Co2 N5 C33 C32 6.3(9) . . . . ? N4 C32 C33 N5 -11.2(10) . . . . ? C31 C32 C33 N5 171.1(8) . . . . ? N4 C32 C33 C34 165.5(7) . . . . ? C31 C32 C33 C34 -12.2(13) . . . . ? N5 C33 C34 C35 -0.1(14) . . . . ? C32 C33 C34 C35 -176.4(8) . . . . ? C33 C34 C35 C36 -0.5(14) . . . . ? C34 C35 C36 C37 1.2(15) . . . . ? C33 N5 C37 C36 0.6(11) . . . . ? Co2 N5 C37 C36 171.6(6) . . . . ? C33 N5 C37 C38 178.4(7) . . . . ? Co2 N5 C37 C38 -10.6(9) . . . . ? C35 C36 C37 N5 -1.3(13) . . . . ? C35 C36 C37 C38 -178.8(9) . . . . ? C40 N6 C38 C37 -177.4(7) . . . . ? Co2 N6 C38 C37 3.7(9) . . . . ? C40 N6 C38 C39 3.4(13) . . . . ? Co2 N6 C38 C39 -175.5(7) . . . . ? N5 C37 C38 N6 3.9(11) . . . . ? C36 C37 C38 N6 -178.5(8) . . . . ? N5 C37 C38 C39 -176.9(7) . . . . ? C36 C37 C38 C39 0.7(13) . . . . ? C38 N6 C40 C45 95.4(10) . . . . ? Co2 N6 C40 C45 -85.8(9) . . . . ? C38 N6 C40 C41 -84.3(11) . . . . ? Co2 N6 C40 C41 94.5(9) . . . . ? N6 C40 C41 C42 -175.6(8) . . . . ? C45 C40 C41 C42 4.7(12) . . . . ? N6 C40 C41 C46 1.9(13) . . . . ? C45 C40 C41 C46 -177.8(7) . . . . ? C40 C41 C42 C43 -3.9(13) . . . . ? C46 C41 C42 C43 178.6(8) . . . . ? C41 C42 C43 C44 3.5(14) . . . . ? C41 C42 C43 C49 176.0(8) . . . . ? C42 C43 C44 C45 -4.0(15) . . . . ? C49 C43 C44 C45 -176.5(8) . . . . ? N6 C40 C45 C44 175.0(8) . . . . ? C41 C40 C45 C44 -5.3(13) . . . . ? N6 C40 C45 C52 -3.8(13) . . . . ? C41 C40 C45 C52 175.9(8) . . . . ? C43 C44 C45 C40 5.1(14) . . . . ? C43 C44 C45 C52 -176.0(9) . . . . ? C42 C41 C46 C48 54.5(11) . . . . ? C40 C41 C46 C48 -122.9(9) . . . . ? C42 C41 C46 C47 -63.6(10) . . . . ? C40 C41 C46 C47 119.0(9) . . . . ? C44 C43 C49 C51 -49.5(15) . . . . ? C42 C43 C49 C51 138.3(11) . . . . ? C44 C43 C49 C50 67.0(15) . . . . ? C42 C43 C49 C50 -105.2(14) . . . . ? C40 C45 C52 C54 -98.1(10) . . . . ? C44 C45 C52 C54 83.1(10) . . . . ? C40 C45 C52 C53 137.4(9) . . . . ? C44 C45 C52 C53 -41.4(11) . . . . ? Co1 N7 C55 C56 32(20) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.881 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.123 # Attachment '09032 rev.cif' data_09032 _database_code_depnum_ccdc_archive 'CCDC 733357' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C112 H134 Br6 Co4 N14 O)(Co Br4)18(C H3 CN)' _chemical_formula_sum 'C148 H190 Br10 Co5 N32 O' _chemical_formula_weight 3527.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.391(6) _cell_length_b 16.542(6) _cell_length_c 26.641(10) _cell_angle_alpha 103.258(7) _cell_angle_beta 92.899(7) _cell_angle_gamma 90.486(7) _cell_volume 7020(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 855 _cell_measurement_theta_min 2.608 _cell_measurement_theta_max 23.368 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3590 _exptl_absorpt_coefficient_mu 3.491 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.512 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details ; absorption correction based on 8755 reflections(SADABS);Rint 0.1154 before correction and 0.0387 after. ; _exptl_special_details ; Only small proportion of independent reflections was actually observed. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54642 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.2827 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.79 _diffrn_reflns_theta_max 26.00 _reflns_number_total 27195 _reflns_number_gt 7866 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Disordered MeCN was omitted using the SQUEEZE option of PLATON.The solvent accessible voids are 1940.9 \%A3 with an estimated 822e/cell to be added. 36 solvent MeCN molecules/unit cell accounting for 792e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46,C-34.The hydrogen atoms on the water O1 have been omitted from the model but have been included in all formulae. The isopropyl carbon atoms are disordered and attempts to split these atoms failed .The data was weak and C55 could not be refined as a "decent" ellipsoid Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 27195 _refine_ls_number_parameters 1308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1592 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1308 _refine_ls_goodness_of_fit_ref 0.668 _refine_ls_restrained_S_all 0.668 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.88407(7) 0.34300(6) 0.06665(4) 0.0418(3) Uani 1 1 d . . . Co2 Co 1.04632(7) 0.18640(6) 0.10865(4) 0.0498(3) Uani 1 1 d . . . Br1 Br 0.81144(5) 0.35009(5) -0.01721(3) 0.0497(3) Uani 1 1 d . . . Br2 Br 0.98706(6) 0.31832(5) 0.14450(3) 0.0602(3) Uani 1 1 d . . . Br3 Br 1.17619(6) 0.18567(6) 0.07253(4) 0.0632(3) Uani 1 1 d . . . N1 N 0.7950(4) 0.4130(4) 0.1233(2) 0.0463(19) Uani 1 1 d . . . N2 N 0.9322(4) 0.4616(3) 0.0887(2) 0.0329(16) Uani 1 1 d . . . N3 N 1.0014(4) 0.3359(4) 0.0281(2) 0.0358(17) Uani 1 1 d . . . N4 N 0.9765(4) 0.1579(4) 0.0304(2) 0.0432(19) Uani 1 1 d . . . N5 N 0.9670(4) 0.0936(4) 0.1126(3) 0.0428(19) Uani 1 1 d . . . N6 N 1.0762(5) 0.1560(4) 0.1858(3) 0.051(2) Uani 1 1 d . . . N7 N 0.8171(5) 0.2374(5) 0.0682(3) 0.053(2) Uani 1 1 d . . . C1 C 0.7189(7) 0.3819(5) 0.1390(3) 0.052(3) Uani 1 1 d . . . C2 C 0.7216(8) 0.3450(6) 0.1825(4) 0.070(3) Uani 1 1 d . . . C3 C 0.6520(9) 0.3114(6) 0.1963(5) 0.086(4) Uani 1 1 d . . . H3 H 0.6555 0.2872 0.2254 0.103 Uiso 1 1 calc R . . C4 C 0.5781(9) 0.3108(8) 0.1707(6) 0.097(4) Uani 1 1 d . . . C5 C 0.5783(7) 0.3482(6) 0.1290(5) 0.071(3) Uani 1 1 d . . . H5 H 0.5277 0.3489 0.1102 0.086 Uiso 1 1 calc R . . C6 C 0.6458(7) 0.3850(6) 0.1121(4) 0.061(3) Uani 1 1 d . . . C7 C 0.6384(6) 0.4271(6) 0.0668(4) 0.062(3) Uani 1 1 d . . . H7 H 0.6948 0.4371 0.0565 0.074 Uiso 1 1 calc R . . C8 C 0.5976(6) 0.5114(6) 0.0836(3) 0.086(3) Uani 1 1 d . . . H8A H 0.5420 0.5029 0.0935 0.129 Uiso 1 1 calc R . . H8B H 0.5956 0.5394 0.0549 0.129 Uiso 1 1 calc R . . H8C H 0.6292 0.5458 0.1132 0.129 Uiso 1 1 calc R . . C9 C 0.5910(5) 0.3748(6) 0.0202(4) 0.091(4) Uani 1 1 d . . . H9A H 0.6118 0.3182 0.0127 0.137 Uiso 1 1 calc R . . H9B H 0.5974 0.3991 -0.0097 0.137 Uiso 1 1 calc R . . H9C H 0.5330 0.3733 0.0273 0.137 Uiso 1 1 calc R . . C10 C 0.8055(7) 0.3449(6) 0.2149(4) 0.080(3) Uani 1 1 d . . . H10 H 0.8499 0.3696 0.1985 0.096 Uiso 1 1 calc R . . C11 C 0.7983(7) 0.3961(7) 0.2725(4) 0.123(5) Uani 1 1 d . . . H11A H 0.7842 0.4535 0.2725 0.185 Uiso 1 1 calc R . . H11B H 0.8507 0.3956 0.2919 0.185 Uiso 1 1 calc R . . H11C H 0.7557 0.3708 0.2888 0.185 Uiso 1 1 calc R . . C12 C 0.8279(7) 0.2544(6) 0.2181(4) 0.101(4) Uani 1 1 d . . . H12A H 0.8792 0.2556 0.2388 0.152 Uiso 1 1 calc R . . H12B H 0.8343 0.2205 0.1832 0.152 Uiso 1 1 calc R . . H12C H 0.7842 0.2303 0.2342 0.152 Uiso 1 1 calc R . . C13 C 0.5051(8) 0.2689(7) 0.1899(6) 0.114(5) Uani 1 1 d . . . H13 H 0.5030 0.2946 0.2276 0.137 Uiso 1 1 calc R . . C14 C 0.4293(8) 0.2866(7) 0.1664(5) 0.132(5) Uani 1 1 d . . . H14A H 0.4248 0.3468 0.1706 0.199 Uiso 1 1 calc R . . H14B H 0.3842 0.2657 0.1830 0.199 Uiso 1 1 calc R . . H14C H 0.4269 0.2595 0.1296 0.199 Uiso 1 1 calc R . . C15 C 0.5248(9) 0.1778(8) 0.1854(7) 0.217(9) Uani 1 1 d . . . H15A H 0.4761 0.1479 0.1919 0.325 Uiso 1 1 calc R . . H15B H 0.5689 0.1735 0.2109 0.325 Uiso 1 1 calc R . . H15C H 0.5422 0.1536 0.1506 0.325 Uiso 1 1 calc R . . C16 C 0.7751(5) 0.5502(5) 0.1816(3) 0.059(3) Uani 1 1 d . . . H16A H 0.7225 0.5259 0.1872 0.089 Uiso 1 1 calc R . . H16B H 0.7656 0.6006 0.1689 0.089 Uiso 1 1 calc R . . H16C H 0.8081 0.5643 0.2143 0.089 Uiso 1 1 calc R . . C17 C 0.8197(6) 0.4885(5) 0.1424(3) 0.045(2) Uani 1 1 d . . . C18 C 0.8947(5) 0.5169(5) 0.1239(3) 0.036(2) Uani 1 1 d . . . C19 C 0.9305(5) 0.5967(5) 0.1417(3) 0.045(2) Uani 1 1 d . . . H19 H 0.9039 0.6375 0.1662 0.054 Uiso 1 1 calc R . . C20 C 1.0008(5) 0.6149(5) 0.1246(3) 0.047(2) Uani 1 1 d . . . H20 H 1.0248 0.6687 0.1368 0.056 Uiso 1 1 calc R . . C21 C 1.0393(5) 0.5564(5) 0.0893(3) 0.044(2) Uani 1 1 d . . . H21 H 1.0903 0.5685 0.0770 0.053 Uiso 1 1 calc R . . C22 C 1.0017(5) 0.4789(5) 0.0720(3) 0.031(2) Uani 1 1 d . . . C23 C 1.0388(5) 0.4103(5) 0.0343(3) 0.036(2) Uani 1 1 d . . . C24 C 1.1042(5) 0.4196(5) 0.0064(3) 0.044(2) Uani 1 1 d . . . H24 H 1.1286 0.4733 0.0112 0.053 Uiso 1 1 calc R . . C25 C 1.1368(5) 0.3550(5) -0.0286(3) 0.046(2) Uani 1 1 d . . . H25 H 1.1831 0.3615 -0.0474 0.055 Uiso 1 1 calc R . . C26 C 1.0964(6) 0.2803(6) -0.0337(3) 0.055(3) Uani 1 1 d . . . H26 H 1.1147 0.2333 -0.0579 0.066 Uiso 1 1 calc R . . C27 C 1.0309(5) 0.2702(5) -0.0056(3) 0.034(2) Uani 1 1 d . . . C28 C 0.9877(5) 0.1880(5) -0.0111(4) 0.044(2) Uani 1 1 d . . . C29 C 0.9606(6) 0.1487(5) -0.0627(3) 0.060(3) Uani 1 1 d . . . H29 H 0.9717 0.1717 -0.0912 0.072 Uiso 1 1 calc R . . C30 C 0.9179(6) 0.0762(6) -0.0683(4) 0.070(3) Uani 1 1 d . . . H30 H 0.9004 0.0457 -0.1019 0.084 Uiso 1 1 calc R . . C31 C 0.8995(5) 0.0462(5) -0.0258(4) 0.053(3) Uani 1 1 d . . . H31 H 0.8659 -0.0022 -0.0300 0.063 Uiso 1 1 calc R . . C32 C 0.9307(5) 0.0876(5) 0.0242(3) 0.048(2) Uani 1 1 d . . . C33 C 0.9172(6) 0.0580(5) 0.0716(3) 0.047(2) Uani 1 1 d . . . C34 C 0.8578(6) -0.0002(5) 0.0753(4) 0.058(3) Uani 1 1 d . . . H34 H 0.8227 -0.0245 0.0462 0.070 Uiso 1 1 calc R . . C35 C 0.8504(6) -0.0217(6) 0.1205(4) 0.063(3) Uani 1 1 d . . . H35 H 0.8100 -0.0616 0.1236 0.076 Uiso 1 1 calc R . . C36 C 0.9008(6) 0.0140(5) 0.1618(4) 0.055(3) Uani 1 1 d . . . H36 H 0.8957 -0.0002 0.1941 0.066 Uiso 1 1 calc R . . C37 C 0.9595(6) 0.0711(5) 0.1563(3) 0.045(2) Uani 1 1 d . . . C38 C 1.0220(6) 0.1093(5) 0.1980(4) 0.051(3) Uani 1 1 d . . . C39 C 1.0208(5) 0.0845(5) 0.2492(3) 0.065(3) Uani 1 1 d . . . H39A H 1.0744 0.0967 0.2676 0.098 Uiso 1 1 calc R . . H39B H 1.0083 0.0249 0.2432 0.098 Uiso 1 1 calc R . . H39C H 0.9789 0.1158 0.2700 0.098 Uiso 1 1 calc R . . C40 C 1.1492(7) 0.1814(6) 0.2218(3) 0.062(3) Uani 1 1 d . . . C41 C 1.1431(8) 0.2525(6) 0.2643(4) 0.100(4) Uani 1 1 d . . . C42 C 1.2085(9) 0.2723(7) 0.3004(4) 0.121(5) Uani 1 1 d . . . H42 H 1.2060 0.3179 0.3293 0.145 Uiso 1 1 calc R . . C43 C 1.2794(10) 0.2229(8) 0.2930(6) 0.121(6) Uani 1 1 d . . . C44 C 1.2836(7) 0.1564(7) 0.2496(4) 0.083(4) Uani 1 1 d . . . H44 H 1.3318 0.1248 0.2439 0.100 Uiso 1 1 calc R . . C45 C 1.2177(7) 0.1381(6) 0.2160(4) 0.061(3) Uani 1 1 d . . . C46 C 1.0639(9) 0.3064(7) 0.2764(5) 0.140(6) Uani 1 1 d . . . H46 H 1.0212 0.2830 0.2486 0.168 Uiso 1 1 calc R . . C47 C 1.0286(10) 0.3005(8) 0.3289(4) 0.181(8) Uani 1 1 d . . . H47A H 1.0289 0.2426 0.3320 0.272 Uiso 1 1 calc R . . H47B H 0.9725 0.3205 0.3302 0.272 Uiso 1 1 calc R . . H47C H 1.0624 0.3348 0.3575 0.272 Uiso 1 1 calc R . . C48 C 1.0916(10) 0.3994(6) 0.2684(5) 0.204(9) Uani 1 1 d . . . H48A H 1.0432 0.4339 0.2686 0.306 Uiso 1 1 calc R . . H48B H 1.1172 0.3931 0.2353 0.306 Uiso 1 1 calc R . . H48C H 1.1305 0.4260 0.2966 0.306 Uiso 1 1 calc R . . C49 C 1.3577(12) 0.2434(10) 0.3345(7) 0.201(10) Uani 1 1 d . . . H49 H 1.3350 0.2886 0.3614 0.241 Uiso 1 1 calc R . . C50 C 1.4173(13) 0.2809(16) 0.3224(9) 0.38(2) Uani 1 1 d . . . H50A H 1.4676 0.2520 0.3283 0.572 Uiso 1 1 calc R . . H50B H 1.4205 0.3378 0.3437 0.572 Uiso 1 1 calc R . . H50C H 1.4107 0.2823 0.2859 0.572 Uiso 1 1 calc R . . C51 C 1.3643(8) 0.1762(8) 0.3631(5) 0.156(6) Uani 1 1 d . . . H51A H 1.4052 0.1925 0.3919 0.234 Uiso 1 1 calc R . . H51B H 1.3810 0.1249 0.3398 0.234 Uiso 1 1 calc R . . H51C H 1.3113 0.1671 0.3765 0.234 Uiso 1 1 calc R . . C52 C 1.2237(5) 0.0637(7) 0.1709(4) 0.070(3) Uani 1 1 d . . . H52 H 1.1803 0.0690 0.1441 0.083 Uiso 1 1 calc R . . C53 C 1.3059(6) 0.0579(6) 0.1452(4) 0.095(4) Uani 1 1 d . . . H53A H 1.3191 0.1111 0.1370 0.142 Uiso 1 1 calc R . . H53B H 1.3022 0.0141 0.1133 0.142 Uiso 1 1 calc R . . H53C H 1.3488 0.0446 0.1688 0.142 Uiso 1 1 calc R . . C54 C 1.2064(5) -0.0197(5) 0.1875(4) 0.076(3) Uani 1 1 d . . . H54A H 1.2466 -0.0254 0.2149 0.114 Uiso 1 1 calc R . . H54B H 1.2106 -0.0666 0.1577 0.114 Uiso 1 1 calc R . . H54C H 1.1513 -0.0190 0.2002 0.114 Uiso 1 1 calc R . . C55 C 0.7607(7) 0.2006(6) 0.0730(4) 0.068(3) Uani 1 1 d . . . C56 C 0.6872(6) 0.1497(7) 0.0798(4) 0.108(4) Uani 1 1 d . . . H56A H 0.6750 0.1069 0.0480 0.162 Uiso 1 1 calc R . . H56B H 0.6401 0.1859 0.0870 0.162 Uiso 1 1 calc R . . H56C H 0.6985 0.1231 0.1086 0.162 Uiso 1 1 calc R . . Co1A Co 0.21806(9) 0.84656(9) 0.47126(5) 0.0804(5) Uani 1 1 d . . . Co2A Co 0.40962(7) 0.84054(8) 0.30153(5) 0.0616(4) Uani 1 1 d . . . Br1A Br 0.36183(7) 0.82116(7) 0.47467(4) 0.0863(4) Uani 1 1 d . . . Br2A Br 0.17797(7) 0.97592(7) 0.53144(4) 0.0975(4) Uani 1 1 d . . . Br3A Br 0.42443(6) 0.96159(6) 0.25936(4) 0.0754(3) Uani 1 1 d . . . N1A N 0.1887(6) 0.7466(6) 0.5109(3) 0.085(3) Uani 1 1 d . . . N2A N 0.1000(5) 0.8105(6) 0.4460(3) 0.076(3) Uani 1 1 d . . . N3A N 0.1976(5) 0.8997(5) 0.4016(3) 0.061(2) Uani 1 1 d . . . N4A N 0.3973(5) 0.9336(4) 0.3776(3) 0.059(2) Uani 1 1 d . . . N5A N 0.5289(5) 0.8577(5) 0.3305(3) 0.065(2) Uani 1 1 d . . . N6A N 0.4813(5) 0.7424(4) 0.2507(3) 0.061(2) Uani 1 1 d . . . N7A N 0.3029(5) 0.7963(5) 0.2575(3) 0.071(3) Uani 1 1 d . . . O1 O 0.3780(3) 0.7516(3) 0.3460(2) 0.0675(18) Uani 1 1 d . . . C1A C 0.2410(7) 0.6965(8) 0.5357(5) 0.097(4) Uani 1 1 d . . . C2A C 0.2556(8) 0.6155(8) 0.5090(4) 0.102(4) Uani 1 1 d . . . C3A C 0.3088(7) 0.5697(8) 0.5339(4) 0.119(5) Uani 1 1 d . . . H3A H 0.3197 0.5141 0.5169 0.143 Uiso 1 1 calc R . . C4A C 0.3466(8) 0.6022(9) 0.5828(5) 0.111(4) Uani 1 1 d . . . C5A C 0.3266(8) 0.6830(7) 0.6077(4) 0.103(4) Uani 1 1 d . . . H5A H 0.3496 0.7050 0.6416 0.124 Uiso 1 1 calc R . . C6A C 0.2747(8) 0.7331(7) 0.5856(4) 0.089(4) Uani 1 1 d . . . C7A C 0.2554(8) 0.8163(6) 0.6130(4) 0.096(4) Uani 1 1 d . . . H7A H 0.2342 0.8474 0.5871 0.115 Uiso 1 1 calc R . . C8A C 0.1879(10) 0.8116(7) 0.6500(5) 0.169(7) Uani 1 1 d . . . H8A1 H 0.1371 0.7909 0.6301 0.253 Uiso 1 1 calc R . . H8A2 H 0.1794 0.8670 0.6716 0.253 Uiso 1 1 calc R . . H8A3 H 0.2041 0.7737 0.6720 0.253 Uiso 1 1 calc R . . C9A C 0.3340(9) 0.8635(7) 0.6420(5) 0.164(6) Uani 1 1 d . . . H9A1 H 0.3639 0.8271 0.6605 0.246 Uiso 1 1 calc R . . H9A2 H 0.3180 0.9136 0.6668 0.246 Uiso 1 1 calc R . . H9A3 H 0.3691 0.8791 0.6170 0.246 Uiso 1 1 calc R . . C10A C 0.2217(10) 0.5779(10) 0.4531(5) 0.155(7) Uani 1 1 d . . . H10A H 0.1817 0.6170 0.4425 0.186 Uiso 1 1 calc R . . C11A C 0.2890(7) 0.5639(8) 0.4164(4) 0.129(5) Uani 1 1 d . . . H11D H 0.3117 0.6176 0.4135 0.193 Uiso 1 1 calc R . . H11E H 0.2674 0.5331 0.3823 0.193 Uiso 1 1 calc R . . H11F H 0.3321 0.5318 0.4292 0.193 Uiso 1 1 calc R . . C12A C 0.1776(10) 0.4920(11) 0.4498(6) 0.229(11) Uani 1 1 d . . . H12D H 0.1541 0.4705 0.4146 0.344 Uiso 1 1 calc R . . H12E H 0.1340 0.4994 0.4741 0.344 Uiso 1 1 calc R . . H12F H 0.2172 0.4526 0.4584 0.344 Uiso 1 1 calc R . . C13A C 0.4123(15) 0.5510(10) 0.6037(7) 0.192(11) Uani 1 1 d . . . H13A H 0.4333 0.5847 0.6381 0.231 Uiso 1 1 calc R . . C14A C 0.3634(12) 0.4775(11) 0.6136(5) 0.228(10) Uani 1 1 d . . . H14D H 0.3566 0.4342 0.5816 0.341 Uiso 1 1 calc R . . H14E H 0.3096 0.4962 0.6254 0.341 Uiso 1 1 calc R . . H14F H 0.3927 0.4550 0.6402 0.341 Uiso 1 1 calc R . . C15A C 0.4867(11) 0.5196(14) 0.5730(7) 0.239(13) Uani 1 1 d . . . H15D H 0.4694 0.4986 0.5365 0.359 Uiso 1 1 calc R . . H15E H 0.5118 0.4748 0.5864 0.359 Uiso 1 1 calc R . . H15F H 0.5265 0.5653 0.5762 0.359 Uiso 1 1 calc R . . C16A C 0.0654(7) 0.6707(8) 0.5364(4) 0.124(5) Uani 1 1 d . . . H16D H 0.1054 0.6384 0.5517 0.186 Uiso 1 1 calc R . . H16E H 0.0283 0.6328 0.5116 0.186 Uiso 1 1 calc R . . H16F H 0.0338 0.7042 0.5637 0.186 Uiso 1 1 calc R . . C17A C 0.1117(10) 0.7300(7) 0.5075(4) 0.086(4) Uani 1 1 d . . . C18A C 0.0551(9) 0.7698(8) 0.4737(4) 0.086(4) Uani 1 1 d . . . C19A C -0.0312(7) 0.7662(8) 0.4670(5) 0.099(4) Uani 1 1 d . . . H19A H -0.0630 0.7389 0.4873 0.119 Uiso 1 1 calc R . . C20A C -0.0679(9) 0.8026(9) 0.4310(6) 0.118(5) Uani 1 1 d . . . H20A H -0.1258 0.8010 0.4266 0.142 Uiso 1 1 calc R . . C21A C -0.0227(8) 0.8417(8) 0.4006(5) 0.097(4) Uani 1 1 d . . . H21A H -0.0482 0.8664 0.3752 0.117 Uiso 1 1 calc R . . C22A C 0.0621(9) 0.8432(7) 0.4090(4) 0.080(4) Uani 1 1 d . . . C23A C 0.1209(7) 0.8830(6) 0.3818(4) 0.060(3) Uani 1 1 d . . . C24A C 0.0945(7) 0.9024(7) 0.3353(4) 0.079(4) Uani 1 1 d . . . H24A H 0.0393 0.8930 0.3224 0.095 Uiso 1 1 calc R . . C25A C 0.1515(7) 0.9355(6) 0.3090(4) 0.078(3) Uani 1 1 d . . . H25A H 0.1365 0.9456 0.2761 0.093 Uiso 1 1 calc R . . C26A C 0.2309(6) 0.9543(5) 0.3301(4) 0.065(3) Uani 1 1 d . . . H26A H 0.2694 0.9804 0.3131 0.078 Uiso 1 1 calc R . . C27A C 0.2516(7) 0.9340(6) 0.3758(4) 0.056(3) Uani 1 1 d . . . C28A C 0.3315(7) 0.9627(6) 0.4009(4) 0.067(3) Uani 1 1 d . . . C29A C 0.3374(7) 1.0241(6) 0.4467(3) 0.076(3) Uani 1 1 d . . . H29A H 0.2901 1.0427 0.4647 0.091 Uiso 1 1 calc R . . C30A C 0.4148(7) 1.0575(6) 0.4655(4) 0.085(4) Uani 1 1 d . . . H30A H 0.4197 1.1024 0.4951 0.102 Uiso 1 1 calc R . . C31A C 0.4832(6) 1.0261(6) 0.4416(4) 0.068(3) Uani 1 1 d . . . H31A H 0.5360 1.0474 0.4545 0.081 Uiso 1 1 calc R . . C32A C 0.4732(7) 0.9640(6) 0.3993(4) 0.067(3) Uani 1 1 d . . . C33A C 0.5451(7) 0.9218(6) 0.3744(4) 0.067(3) Uani 1 1 d . . . C34A C 0.6309(7) 0.9383(8) 0.3894(4) 0.097(4) Uani 1 1 d . . . H34A H 0.6460 0.9806 0.4192 0.117 Uiso 1 1 calc R . . C35A C 0.6912(7) 0.8939(9) 0.3614(5) 0.119(5) Uani 1 1 d . . . H35A H 0.7472 0.9066 0.3713 0.143 Uiso 1 1 calc R . . C36A C 0.6695(7) 0.8310(7) 0.3188(4) 0.093(4) Uani 1 1 d . . . H36A H 0.7099 0.7996 0.2990 0.111 Uiso 1 1 calc R . . C37A C 0.5875(6) 0.8149(7) 0.3059(4) 0.077(3) Uani 1 1 d . . . C38A C 0.5581(6) 0.7478(7) 0.2615(4) 0.071(3) Uani 1 1 d . . . C39A C 0.6198(6) 0.6928(6) 0.2338(3) 0.087(4) Uani 1 1 d . . . H39D H 0.5924 0.6496 0.2066 0.131 Uiso 1 1 calc R . . H39E H 0.6508 0.6669 0.2581 0.131 Uiso 1 1 calc R . . H39F H 0.6571 0.7255 0.2183 0.131 Uiso 1 1 calc R . . C40A C 0.4421(6) 0.6749(7) 0.2118(3) 0.067(3) Uani 1 1 d . . . C41A C 0.4267(7) 0.5964(7) 0.2213(4) 0.075(3) Uani 1 1 d . . . C42A C 0.3816(7) 0.5399(6) 0.1841(4) 0.092(4) Uani 1 1 d . . . H42A H 0.3716 0.4864 0.1901 0.110 Uiso 1 1 calc R . . C43A C 0.3506(7) 0.5559(7) 0.1394(4) 0.086(4) Uani 1 1 d . . . C44A C 0.3699(6) 0.6310(6) 0.1269(4) 0.071(3) Uani 1 1 d . . . H44A H 0.3525 0.6410 0.0944 0.085 Uiso 1 1 calc R . . C45A C 0.4152(6) 0.6913(6) 0.1633(4) 0.067(3) Uani 1 1 d . . . C46A C 0.4588(7) 0.5724(7) 0.2690(4) 0.089(4) Uani 1 1 d . . . H46A H 0.4848 0.6228 0.2926 0.107 Uiso 1 1 calc R . . C47A C 0.5249(7) 0.5061(6) 0.2559(4) 0.112(5) Uani 1 1 d . . . H47D H 0.5035 0.4601 0.2282 0.168 Uiso 1 1 calc R . . H47E H 0.5399 0.4853 0.2866 0.168 Uiso 1 1 calc R . . H47F H 0.5732 0.5309 0.2446 0.168 Uiso 1 1 calc R . . C48A C 0.3884(8) 0.5388(7) 0.2989(4) 0.120(5) Uani 1 1 d . . . H48D H 0.3438 0.5785 0.3040 0.180 Uiso 1 1 calc R . . H48E H 0.4107 0.5322 0.3325 0.180 Uiso 1 1 calc R . . H48F H 0.3674 0.4850 0.2785 0.180 Uiso 1 1 calc R . . C49A C 0.2938(9) 0.4914(7) 0.1004(5) 0.097(4) Uani 1 1 d . . . H49A H 0.2604 0.5247 0.0803 0.116 Uiso 1 1 calc R . . C50A C 0.2347(7) 0.4488(8) 0.1257(5) 0.147(6) Uani 1 1 d . . . H50G H 0.1986 0.4126 0.0994 0.220 Uiso 1 1 calc R . . H50H H 0.2022 0.4901 0.1482 0.220 Uiso 1 1 calc R . . H50I H 0.2641 0.4154 0.1465 0.220 Uiso 1 1 calc R . . C51A C 0.3452(7) 0.4387(7) 0.0626(5) 0.136(6) Uani 1 1 d . . . H51D H 0.3844 0.4096 0.0808 0.204 Uiso 1 1 calc R . . H51E H 0.3747 0.4736 0.0441 0.204 Uiso 1 1 calc R . . H51F H 0.3105 0.3981 0.0380 0.204 Uiso 1 1 calc R . . C52A C 0.4384(8) 0.7718(6) 0.1507(4) 0.094(4) Uani 1 1 d . . . H52A H 0.4537 0.8119 0.1841 0.113 Uiso 1 1 calc R . . C53A C 0.3657(7) 0.8102(6) 0.1243(4) 0.106(4) Uani 1 1 d . . . H53D H 0.3523 0.7751 0.0899 0.159 Uiso 1 1 calc R . . H53E H 0.3814 0.8661 0.1212 0.159 Uiso 1 1 calc R . . H53F H 0.3180 0.8134 0.1453 0.159 Uiso 1 1 calc R . . C54A C 0.5196(7) 0.7616(7) 0.1160(4) 0.120(5) Uani 1 1 d . . . H54D H 0.5669 0.7490 0.1367 0.181 Uiso 1 1 calc R . . H54E H 0.5303 0.8135 0.1054 0.181 Uiso 1 1 calc R . . H54F H 0.5100 0.7163 0.0853 0.181 Uiso 1 1 calc R . . C55A C 0.2566(7) 0.7578(7) 0.2285(5) 0.089(4) Uani 1 1 d . . . C56A C 0.1962(6) 0.7072(6) 0.1899(4) 0.113(5) Uani 1 1 d . . . H56D H 0.1795 0.7385 0.1641 0.169 Uiso 1 1 calc R . . H56E H 0.1482 0.6945 0.2074 0.169 Uiso 1 1 calc R . . H56F H 0.2213 0.6553 0.1727 0.169 Uiso 1 1 calc R . . Co3 Co 0.87768(7) 0.82100(7) 0.23360(4) 0.0510(3) Uani 1 1 d . . . Br4 Br 0.77985(6) 0.78426(5) 0.16029(3) 0.0541(3) Uani 1 1 d . . . Br5 Br 0.85642(6) 0.95161(6) 0.29240(4) 0.0649(3) Uani 1 1 d . . . Br6 Br 1.00991(6) 0.83401(5) 0.19940(3) 0.0582(3) Uani 1 1 d . . . Br7 Br 0.87166(7) 0.71755(6) 0.28471(4) 0.0768(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0578(8) 0.0237(6) 0.0409(7) 0.0028(5) -0.0034(6) 0.0025(6) Co2 0.0730(9) 0.0268(7) 0.0463(8) 0.0034(6) -0.0046(7) 0.0056(6) Br1 0.0553(6) 0.0487(6) 0.0448(6) 0.0119(4) -0.0063(5) -0.0006(5) Br2 0.0916(8) 0.0379(6) 0.0460(6) 0.0016(4) -0.0096(5) 0.0179(5) Br3 0.0741(7) 0.0500(6) 0.0680(7) 0.0215(5) -0.0055(6) -0.0054(6) N1 0.067(6) 0.032(5) 0.038(4) 0.004(4) 0.004(4) 0.014(4) N2 0.047(5) 0.014(4) 0.036(4) 0.004(3) 0.000(4) 0.001(4) N3 0.050(5) 0.018(4) 0.041(4) 0.012(3) -0.013(4) 0.003(4) N4 0.074(6) 0.019(4) 0.036(4) 0.003(3) 0.005(4) 0.007(4) N5 0.060(5) 0.015(4) 0.047(5) -0.005(4) -0.007(4) 0.012(3) N6 0.075(6) 0.029(4) 0.048(5) 0.008(4) -0.002(5) 0.015(4) N7 0.059(6) 0.040(5) 0.064(5) 0.019(4) -0.002(5) 0.006(4) C1 0.074(8) 0.041(6) 0.044(6) 0.011(5) 0.019(6) 0.011(6) C2 0.096(9) 0.039(6) 0.082(8) 0.026(6) 0.016(8) 0.019(6) C3 0.105(10) 0.048(7) 0.116(11) 0.025(7) 0.071(10) 0.009(8) C4 0.087(11) 0.071(9) 0.127(13) 0.010(8) 0.017(10) 0.000(9) C5 0.060(8) 0.050(7) 0.097(9) -0.003(6) 0.021(7) 0.005(6) C6 0.060(8) 0.052(7) 0.063(7) -0.001(6) 0.000(7) 0.002(6) C7 0.049(6) 0.059(7) 0.070(7) -0.002(6) 0.017(6) 0.002(6) C8 0.095(8) 0.091(9) 0.060(7) -0.002(6) -0.015(6) 0.007(7) C9 0.063(7) 0.119(10) 0.069(7) -0.026(7) 0.001(6) 0.013(7) C10 0.129(10) 0.054(7) 0.068(8) 0.028(6) 0.042(8) 0.031(7) C11 0.187(13) 0.092(9) 0.090(9) 0.016(8) 0.011(9) 0.044(9) C12 0.142(11) 0.091(9) 0.085(8) 0.043(7) 0.029(8) 0.038(8) C13 0.092(10) 0.058(9) 0.196(15) 0.032(9) 0.027(11) -0.011(8) C14 0.119(12) 0.083(10) 0.199(15) 0.034(10) 0.033(12) 0.020(9) C15 0.190(16) 0.074(11) 0.39(3) 0.065(14) 0.057(17) -0.028(11) C16 0.061(7) 0.045(6) 0.070(7) 0.011(5) 0.012(6) -0.001(5) C17 0.070(7) 0.020(5) 0.048(6) 0.010(4) 0.008(5) 0.009(5) C18 0.045(6) 0.018(5) 0.043(5) 0.004(4) 0.007(5) 0.001(4) C19 0.041(6) 0.044(6) 0.046(6) -0.001(5) 0.006(5) 0.013(5) C20 0.054(7) 0.031(5) 0.048(6) -0.007(4) -0.001(5) -0.004(5) C21 0.031(5) 0.055(6) 0.045(6) 0.014(5) -0.012(4) 0.001(5) C22 0.039(6) 0.017(5) 0.036(5) 0.005(4) -0.010(4) 0.001(4) C23 0.039(6) 0.036(6) 0.036(5) 0.011(4) 0.007(4) 0.010(5) C24 0.071(7) 0.025(5) 0.033(5) 0.003(4) -0.016(5) 0.007(5) C25 0.059(6) 0.040(6) 0.037(5) 0.004(5) -0.003(5) 0.014(5) C26 0.079(8) 0.041(6) 0.039(6) -0.001(5) -0.008(6) 0.024(6) C27 0.042(6) 0.021(5) 0.039(5) 0.007(4) 0.001(5) 0.010(4) C28 0.050(6) 0.023(5) 0.050(6) -0.013(5) 0.004(5) 0.011(4) C29 0.098(8) 0.024(5) 0.057(7) 0.009(5) -0.007(6) 0.005(6) C30 0.109(9) 0.054(7) 0.039(6) 0.003(5) -0.027(6) 0.018(7) C31 0.062(7) 0.027(5) 0.062(7) -0.002(5) -0.009(6) -0.003(5) C32 0.066(7) 0.021(5) 0.046(6) -0.010(4) -0.010(5) 0.010(5) C33 0.065(7) 0.030(5) 0.045(6) 0.006(5) -0.004(5) 0.008(5) C34 0.081(8) 0.036(6) 0.056(7) 0.007(5) -0.003(6) 0.004(6) C35 0.074(8) 0.059(7) 0.057(7) 0.015(6) -0.004(6) 0.008(6) C36 0.071(7) 0.033(6) 0.059(7) 0.008(5) 0.000(6) 0.010(5) C37 0.069(7) 0.028(5) 0.035(6) 0.005(5) -0.016(5) 0.016(5) C38 0.075(8) 0.021(5) 0.061(7) 0.018(5) 0.013(6) 0.021(5) C39 0.089(8) 0.059(7) 0.045(6) 0.008(5) -0.002(6) 0.009(6) C40 0.102(9) 0.033(6) 0.050(6) 0.012(5) -0.027(7) -0.012(6) C41 0.154(12) 0.048(7) 0.084(9) 0.000(6) -0.056(9) 0.012(8) C42 0.211(16) 0.063(9) 0.074(8) 0.009(7) -0.090(10) -0.026(10) C43 0.172(15) 0.057(9) 0.143(13) 0.059(9) -0.077(12) -0.047(9) C44 0.090(9) 0.062(8) 0.091(9) 0.013(7) -0.044(7) -0.018(7) C45 0.073(8) 0.044(7) 0.065(7) 0.016(6) -0.027(6) -0.005(6) C46 0.199(15) 0.068(9) 0.133(13) 0.000(9) -0.092(12) 0.037(10) C47 0.30(2) 0.186(16) 0.035(8) -0.012(9) -0.004(10) 0.106(14) C48 0.37(2) 0.041(8) 0.163(13) -0.021(8) -0.165(15) 0.041(11) C49 0.28(2) 0.135(14) 0.191(17) 0.088(12) -0.187(18) -0.133(15) C50 0.32(3) 0.44(4) 0.40(4) 0.19(3) -0.25(3) -0.31(3) C51 0.214(16) 0.108(11) 0.123(12) 0.007(9) -0.116(11) -0.009(11) C52 0.024(6) 0.099(9) 0.099(9) 0.052(8) 0.000(6) -0.012(6) C53 0.071(8) 0.096(9) 0.131(10) 0.061(8) -0.013(8) -0.023(7) C54 0.064(7) 0.071(7) 0.104(8) 0.049(7) -0.029(6) -0.010(6) C55 0.073(9) 0.047(8) 0.081(8) 0.010(6) -0.006(8) 0.024(6) C56 0.084(9) 0.089(9) 0.152(12) 0.033(8) 0.000(8) -0.027(8) Co1A 0.0806(11) 0.1012(12) 0.0461(9) -0.0080(8) -0.0079(8) 0.0103(9) Co2A 0.0595(9) 0.0672(9) 0.0463(8) -0.0080(7) -0.0142(7) 0.0053(7) Br1A 0.0858(8) 0.0956(9) 0.0660(7) -0.0005(6) -0.0168(7) 0.0044(7) Br2A 0.1156(10) 0.0977(9) 0.0586(7) -0.0219(6) -0.0087(7) 0.0202(8) Br3A 0.0814(8) 0.0744(8) 0.0615(7) 0.0008(6) -0.0158(6) 0.0075(6) N1A 0.073(7) 0.099(8) 0.066(6) -0.016(5) -0.009(6) 0.004(7) N2A 0.097(8) 0.085(7) 0.030(5) -0.015(5) -0.007(6) 0.000(6) N3A 0.055(6) 0.067(6) 0.040(5) -0.029(4) -0.005(5) 0.016(5) N4A 0.064(6) 0.064(6) 0.037(5) -0.010(4) -0.014(5) 0.008(5) N5A 0.058(6) 0.078(6) 0.047(5) -0.010(5) -0.011(5) -0.001(5) N6A 0.080(6) 0.056(5) 0.036(5) -0.010(4) 0.000(5) 0.010(5) N7A 0.061(6) 0.070(6) 0.072(6) 0.001(5) -0.022(5) 0.007(5) O1 0.075(4) 0.065(4) 0.048(4) -0.017(3) 0.006(3) 0.006(4) C1A 0.102(10) 0.106(10) 0.071(9) 0.000(8) -0.013(8) 0.041(8) C2A 0.121(11) 0.105(10) 0.062(8) -0.015(7) -0.014(7) 0.056(9) C3A 0.124(11) 0.117(11) 0.079(9) -0.046(8) -0.041(8) 0.044(9) C4A 0.138(12) 0.103(11) 0.078(9) 0.005(8) -0.043(9) 0.014(9) C5A 0.158(12) 0.063(8) 0.068(8) -0.019(7) -0.043(8) 0.015(8) C6A 0.143(11) 0.087(9) 0.031(6) 0.004(6) -0.019(7) -0.001(8) C7A 0.168(13) 0.044(7) 0.065(8) -0.006(6) -0.013(9) 0.006(8) C8A 0.28(2) 0.080(10) 0.133(13) -0.015(9) 0.075(14) 0.057(12) C9A 0.231(17) 0.084(10) 0.145(13) -0.026(9) -0.048(13) -0.019(11) C10A 0.163(15) 0.195(17) 0.058(9) -0.065(10) -0.044(9) 0.099(13) C11A 0.161(13) 0.159(13) 0.056(8) 0.003(8) -0.001(9) 0.049(11) C12A 0.186(18) 0.24(2) 0.189(18) -0.080(16) -0.098(15) 0.011(16) C13A 0.35(3) 0.097(13) 0.123(16) 0.050(12) -0.122(18) -0.032(17) C14A 0.39(3) 0.178(18) 0.105(13) 0.024(13) -0.096(16) 0.09(2) C15A 0.25(2) 0.31(3) 0.164(19) 0.052(18) 0.006(17) 0.12(2) C16A 0.118(11) 0.141(12) 0.094(10) -0.005(9) -0.022(9) 0.001(10) C17A 0.141(13) 0.065(8) 0.037(7) -0.017(6) 0.011(9) -0.003(9) C18A 0.105(12) 0.103(10) 0.038(7) -0.005(7) -0.021(8) 0.025(9) C19A 0.055(9) 0.153(13) 0.077(9) 0.001(8) -0.006(7) 0.010(8) C20A 0.088(11) 0.151(14) 0.093(12) -0.012(10) -0.021(10) 0.038(10) C21A 0.073(11) 0.138(13) 0.059(9) -0.019(8) -0.009(8) 0.005(9) C22A 0.089(11) 0.092(9) 0.042(7) -0.021(6) 0.004(8) 0.026(8) C23A 0.071(8) 0.067(7) 0.028(6) -0.020(5) -0.004(6) 0.017(6) C24A 0.066(8) 0.108(10) 0.051(7) -0.006(7) -0.012(6) 0.027(7) C25A 0.093(10) 0.079(8) 0.052(7) 0.000(6) -0.006(7) 0.032(7) C26A 0.063(7) 0.067(7) 0.058(7) 0.006(6) -0.018(6) 0.007(6) C27A 0.069(8) 0.055(7) 0.031(6) -0.017(5) -0.003(6) 0.017(6) C28A 0.065(8) 0.072(8) 0.045(6) -0.020(5) -0.010(6) 0.016(6) C29A 0.098(9) 0.065(7) 0.049(7) -0.016(6) -0.004(6) 0.014(7) C30A 0.107(10) 0.077(8) 0.055(7) -0.010(6) -0.035(7) -0.035(8) C31A 0.069(8) 0.066(8) 0.051(7) -0.016(6) -0.009(6) 0.003(6) C32A 0.080(8) 0.065(7) 0.048(7) -0.005(6) -0.009(6) 0.010(7) C33A 0.086(9) 0.065(7) 0.045(6) 0.003(5) -0.006(6) 0.000(7) C34A 0.080(9) 0.145(12) 0.059(8) 0.020(8) -0.042(7) -0.061(9) C35A 0.045(8) 0.222(17) 0.085(10) 0.017(10) 0.022(8) 0.020(9) C36A 0.073(9) 0.145(11) 0.039(7) -0.019(7) -0.008(6) -0.020(8) C37A 0.042(7) 0.119(10) 0.061(8) 0.003(7) -0.008(6) -0.001(7) C38A 0.049(7) 0.107(9) 0.044(6) -0.008(6) -0.014(6) 0.013(7) C39A 0.075(8) 0.128(10) 0.050(7) -0.001(6) 0.013(6) 0.019(7) C40A 0.085(8) 0.072(8) 0.037(6) 0.002(6) -0.007(6) 0.024(7) C41A 0.104(9) 0.078(8) 0.045(7) 0.018(6) -0.010(6) 0.033(7) C42A 0.156(12) 0.047(7) 0.060(8) -0.004(6) -0.038(8) 0.019(7) C43A 0.125(10) 0.052(8) 0.066(8) -0.013(6) -0.034(7) 0.012(7) C44A 0.101(9) 0.043(7) 0.058(7) -0.005(6) -0.029(6) 0.006(6) C45A 0.101(9) 0.037(6) 0.061(7) 0.005(5) -0.009(6) 0.023(6) C46A 0.130(11) 0.087(9) 0.050(7) 0.015(6) -0.012(7) 0.045(8) C47A 0.157(11) 0.107(9) 0.075(8) 0.030(7) -0.004(8) 0.093(9) C48A 0.170(13) 0.131(11) 0.060(8) 0.025(8) -0.015(9) 0.071(10) C49A 0.147(13) 0.053(8) 0.091(10) 0.024(7) -0.017(9) 0.005(9) C50A 0.111(12) 0.146(14) 0.159(14) 0.005(11) -0.079(11) -0.012(10) C51A 0.114(11) 0.123(11) 0.128(11) -0.050(9) -0.056(9) 0.021(9) C52A 0.142(12) 0.058(8) 0.064(8) -0.013(6) -0.057(8) 0.006(8) C53A 0.160(12) 0.054(7) 0.089(9) -0.006(6) -0.036(8) 0.007(8) C54A 0.122(11) 0.111(11) 0.116(11) 0.009(9) -0.022(9) -0.018(9) C55A 0.068(8) 0.072(8) 0.104(10) -0.026(7) -0.025(7) 0.027(7) C56A 0.074(8) 0.107(9) 0.107(9) -0.069(7) -0.041(7) 0.008(7) Co3 0.0629(9) 0.0366(7) 0.0453(7) -0.0054(6) -0.0073(7) 0.0059(6) Br4 0.0654(7) 0.0434(6) 0.0481(6) 0.0023(5) -0.0099(5) 0.0023(5) Br5 0.0800(7) 0.0489(6) 0.0544(6) -0.0131(5) 0.0099(6) 0.0057(6) Br6 0.0585(6) 0.0450(6) 0.0591(6) -0.0112(5) -0.0031(5) 0.0048(5) Br7 0.1111(9) 0.0615(7) 0.0541(7) 0.0116(5) -0.0234(6) -0.0063(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 2.053(6) . ? Co1 N7 2.064(8) . ? Co1 N3 2.218(7) . ? Co1 N1 2.280(7) . ? Co1 Br1 2.5052(15) . ? Co1 Br2 2.7139(15) . ? Co2 N5 2.028(7) . ? Co2 N6 2.257(7) . ? Co2 N4 2.274(7) . ? Co2 Br3 2.3790(18) . ? Co2 Br2 2.4066(15) . ? N1 C17 1.289(9) . ? N1 C1 1.463(10) . ? N2 C22 1.296(9) . ? N2 C18 1.331(8) . ? N3 C23 1.341(9) . ? N3 C27 1.351(9) . ? N4 C28 1.333(9) . ? N4 C32 1.352(9) . ? N5 C37 1.312(9) . ? N5 C33 1.348(9) . ? N6 C38 1.274(10) . ? N6 C40 1.490(10) . ? N7 C55 1.132(11) . ? C1 C6 1.371(11) . ? C1 C2 1.428(12) . ? C2 C3 1.368(12) . ? C2 C10 1.586(13) . ? C3 C4 1.359(14) . ? C3 H3 0.9500 . ? C4 C5 1.390(14) . ? C4 C13 1.543(16) . ? C5 C6 1.401(12) . ? C5 H5 0.9500 . ? C6 C7 1.526(12) . ? C7 C9 1.515(11) . ? C7 C8 1.534(11) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.565(11) . ? C10 C11 1.585(12) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.424(14) . ? C13 C15 1.523(14) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.506(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.459(10) . ? C18 C19 1.408(10) . ? C19 C20 1.318(10) . ? C19 H19 0.9500 . ? C20 C21 1.369(10) . ? C20 H20 0.9500 . ? C21 C22 1.386(10) . ? C21 H21 0.9500 . ? C22 C23 1.489(10) . ? C23 C24 1.363(10) . ? C24 C25 1.378(10) . ? C24 H24 0.9500 . ? C25 C26 1.373(10) . ? C25 H25 0.9500 . ? C26 C27 1.370(10) . ? C26 H26 0.9500 . ? C27 C28 1.501(10) . ? C28 C29 1.426(10) . ? C29 C30 1.357(11) . ? C29 H29 0.9500 . ? C30 C31 1.384(11) . ? C30 H30 0.9500 . ? C31 C32 1.417(10) . ? C31 H31 0.9500 . ? C32 C33 1.480(11) . ? C33 C34 1.387(11) . ? C34 C35 1.342(11) . ? C34 H34 0.9500 . ? C35 C36 1.359(11) . ? C35 H35 0.9500 . ? C36 C37 1.378(11) . ? C36 H36 0.9500 . ? C37 C38 1.494(11) . ? C38 C39 1.514(10) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C45 1.333(12) . ? C40 C41 1.441(12) . ? C41 C42 1.388(13) . ? C41 C46 1.585(15) . ? C42 C43 1.423(16) . ? C42 H42 0.9500 . ? C43 C44 1.407(15) . ? C43 C49 1.631(16) . ? C44 C45 1.353(11) . ? C44 H44 0.9500 . ? C45 C52 1.518(12) . ? C46 C47 1.564(17) . ? C46 C48 1.664(16) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.25(2) . ? C49 C51 1.487(16) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.535(11) . ? C52 C54 1.570(11) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.506(13) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? Co1A N2A 2.053(9) . ? Co1A N1A 2.218(11) . ? Co1A N3A 2.242(8) . ? Co1A Br1A 2.398(2) . ? Co1A Br2A 2.4775(18) . ? Co2A N5A 2.058(7) . ? Co2A N7A 2.086(8) . ? Co2A O1 2.165(6) . ? Co2A N6A 2.243(7) . ? Co2A N4A 2.266(7) . ? Co2A Br3A 2.5263(19) . ? N1A C17A 1.282(13) . ? N1A C1A 1.437(13) . ? N2A C18A 1.347(13) . ? N2A C22A 1.355(12) . ? N3A C23A 1.339(11) . ? N3A C27A 1.344(11) . ? N4A C28A 1.312(10) . ? N4A C32A 1.384(11) . ? N5A C37A 1.309(10) . ? N5A C33A 1.400(10) . ? N6A C38A 1.275(10) . ? N6A C40A 1.457(11) . ? N7A C55A 1.134(10) . ? C1A C2A 1.395(13) . ? C1A C6A 1.410(13) . ? C2A C3A 1.399(13) . ? C2A C10A 1.548(14) . ? C3A C4A 1.400(13) . ? C3A H3A 0.9500 . ? C4A C5A 1.399(13) . ? C4A C13A 1.535(19) . ? C5A C6A 1.394(13) . ? C5A H5A 0.9500 . ? C6A C7A 1.449(13) . ? C7A C8A 1.533(15) . ? C7A C9A 1.572(14) . ? C7A H7A 1.0000 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A C11A 1.496(16) . ? C10A C12A 1.57(2) . ? C10A H10A 1.0000 . ? C11A H11D 0.9800 . ? C11A H11E 0.9800 . ? C11A H11F 0.9800 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13A C14A 1.53(2) . ? C13A C15A 1.53(2) . ? C13A H13A 1.0000 . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C15A H15D 0.9800 . ? C15A H15E 0.9800 . ? C15A H15F 0.9800 . ? C16A C17A 1.590(14) . ? C16A H16D 0.9800 . ? C16A H16E 0.9800 . ? C16A H16F 0.9800 . ? C17A C18A 1.518(15) . ? C18A C19A 1.416(14) . ? C19A C20A 1.363(15) . ? C19A H19A 0.9500 . ? C20A C21A 1.383(15) . ? C20A H20A 0.9500 . ? C21A C22A 1.396(14) . ? C21A H21A 0.9500 . ? C22A C23A 1.473(14) . ? C23A C24A 1.397(12) . ? C24A C25A 1.377(12) . ? C24A H24A 0.9500 . ? C25A C26A 1.395(12) . ? C25A H25A 0.9500 . ? C26A C27A 1.363(11) . ? C26A H26A 0.9500 . ? C27A C28A 1.462(12) . ? C28A C29A 1.396(11) . ? C29A C30A 1.400(12) . ? C29A H29A 0.9500 . ? C30A C31A 1.365(12) . ? C30A H30A 0.9500 . ? C31A C32A 1.342(11) . ? C31A H31A 0.9500 . ? C32A C33A 1.482(12) . ? C33A C34A 1.448(12) . ? C34A C35A 1.382(13) . ? C34A H34A 0.9500 . ? C35A C36A 1.382(14) . ? C35A H35A 0.9500 . ? C36A C37A 1.377(12) . ? C36A H36A 0.9500 . ? C37A C38A 1.482(13) . ? C38A C39A 1.475(11) . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 0.9800 . ? C40A C41A 1.402(13) . ? C40A C45A 1.429(11) . ? C41A C42A 1.376(12) . ? C41A C46A 1.487(12) . ? C42A C43A 1.354(12) . ? C42A H42A 0.9500 . ? C43A C44A 1.395(13) . ? C43A C49A 1.569(14) . ? C44A C45A 1.400(11) . ? C44A H44A 0.9500 . ? C45A C52A 1.497(13) . ? C46A C47A 1.543(11) . ? C46A C48A 1.601(14) . ? C46A H46A 1.0000 . ? C47A H47D 0.9800 . ? C47A H47E 0.9800 . ? C47A H47F 0.9800 . ? C48A H48D 0.9800 . ? C48A H48E 0.9800 . ? C48A H48F 0.9800 . ? C49A C50A 1.471(14) . ? C49A C51A 1.474(14) . ? C49A H49A 1.0000 . ? C50A H50G 0.9800 . ? C50A H50H 0.9800 . ? C50A H50I 0.9800 . ? C51A H51D 0.9800 . ? C51A H51E 0.9800 . ? C51A H51F 0.9800 . ? C52A C53A 1.565(12) . ? C52A C54A 1.646(14) . ? C52A H52A 1.0000 . ? C53A H53D 0.9800 . ? C53A H53E 0.9800 . ? C53A H53F 0.9800 . ? C54A H54D 0.9800 . ? C54A H54E 0.9800 . ? C54A H54F 0.9800 . ? C55A C56A 1.492(12) . ? C56A H56D 0.9800 . ? C56A H56E 0.9800 . ? C56A H56F 0.9800 . ? Co3 Br5 2.3998(15) . ? Co3 Br6 2.4198(17) . ? Co3 Br7 2.4230(17) . ? Co3 Br4 2.4243(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N7 160.3(3) . . ? N2 Co1 N3 75.8(3) . . ? N7 Co1 N3 121.5(3) . . ? N2 Co1 N1 75.5(3) . . ? N7 Co1 N1 86.2(3) . . ? N3 Co1 N1 151.0(3) . . ? N2 Co1 Br1 99.95(16) . . ? N7 Co1 Br1 90.3(2) . . ? N3 Co1 Br1 88.85(15) . . ? N1 Co1 Br1 100.15(16) . . ? N2 Co1 Br2 82.65(16) . . ? N7 Co1 Br2 90.9(2) . . ? N3 Co1 Br2 80.26(15) . . ? N1 Co1 Br2 91.98(16) . . ? Br1 Co1 Br2 167.87(5) . . ? N5 Co2 N6 74.5(3) . . ? N5 Co2 N4 76.0(3) . . ? N6 Co2 N4 150.2(3) . . ? N5 Co2 Br3 132.12(17) . . ? N6 Co2 Br3 103.2(2) . . ? N4 Co2 Br3 93.79(19) . . ? N5 Co2 Br2 109.44(17) . . ? N6 Co2 Br2 94.88(16) . . ? N4 Co2 Br2 98.33(15) . . ? Br3 Co2 Br2 118.35(6) . . ? Co2 Br2 Co1 103.38(5) . . ? C17 N1 C1 120.5(7) . . ? C17 N1 Co1 111.5(6) . . ? C1 N1 Co1 128.0(5) . . ? C22 N2 C18 121.5(7) . . ? C22 N2 Co1 119.8(5) . . ? C18 N2 Co1 118.4(6) . . ? C23 N3 C27 118.7(7) . . ? C23 N3 Co1 112.8(5) . . ? C27 N3 Co1 127.6(6) . . ? C28 N4 C32 117.9(7) . . ? C28 N4 Co2 129.8(6) . . ? C32 N4 Co2 110.5(5) . . ? C37 N5 C33 118.8(8) . . ? C37 N5 Co2 120.4(6) . . ? C33 N5 Co2 120.6(6) . . ? C38 N6 C40 118.4(8) . . ? C38 N6 Co2 112.6(6) . . ? C40 N6 Co2 129.0(6) . . ? C55 N7 Co1 155.8(8) . . ? C6 C1 C2 119.5(10) . . ? C6 C1 N1 121.7(9) . . ? C2 C1 N1 118.8(10) . . ? C3 C2 C1 119.9(11) . . ? C3 C2 C10 120.8(11) . . ? C1 C2 C10 119.3(10) . . ? C4 C3 C2 123.6(13) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C3 C4 C5 114.4(13) . . ? C3 C4 C13 118.0(14) . . ? C5 C4 C13 127.6(14) . . ? C4 C5 C6 126.4(12) . . ? C4 C5 H5 116.8 . . ? C6 C5 H5 116.8 . . ? C1 C6 C5 116.2(10) . . ? C1 C6 C7 121.8(10) . . ? C5 C6 C7 122.0(10) . . ? C9 C7 C6 112.9(8) . . ? C9 C7 C8 109.5(8) . . ? C6 C7 C8 109.8(7) . . ? C9 C7 H7 108.2 . . ? C6 C7 H7 108.2 . . ? C8 C7 H7 108.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 106.5(8) . . ? C12 C10 C2 110.6(9) . . ? C11 C10 C2 110.6(9) . . ? C12 C10 H10 109.7 . . ? C11 C10 H10 109.7 . . ? C2 C10 H10 109.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 117.2(12) . . ? C14 C13 C4 111.9(12) . . ? C15 C13 C4 107.9(11) . . ? C14 C13 H13 106.4 . . ? C15 C13 H13 106.4 . . ? C4 C13 H13 106.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C18 118.0(8) . . ? N1 C17 C16 124.3(8) . . ? C18 C17 C16 117.7(7) . . ? N2 C18 C19 118.6(8) . . ? N2 C18 C17 116.5(7) . . ? C19 C18 C17 124.8(8) . . ? C20 C19 C18 120.2(8) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 120.1(8) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C22 118.2(8) . . ? C20 C21 H21 120.9 . . ? C22 C21 H21 120.9 . . ? N2 C22 C21 121.4(7) . . ? N2 C22 C23 116.0(7) . . ? C21 C22 C23 122.6(8) . . ? N3 C23 C24 120.5(8) . . ? N3 C23 C22 114.8(7) . . ? C24 C23 C22 124.6(8) . . ? C23 C24 C25 123.3(8) . . ? C23 C24 H24 118.3 . . ? C25 C24 H24 118.3 . . ? C26 C25 C24 114.0(8) . . ? C26 C25 H25 123.0 . . ? C24 C25 H25 123.0 . . ? C27 C26 C25 123.1(8) . . ? C27 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? N3 C27 C26 120.2(8) . . ? N3 C27 C28 117.0(7) . . ? C26 C27 C28 122.7(8) . . ? N4 C28 C29 125.3(8) . . ? N4 C28 C27 120.2(8) . . ? C29 C28 C27 114.5(8) . . ? C30 C29 C28 115.6(9) . . ? C30 C29 H29 122.2 . . ? C28 C29 H29 122.2 . . ? C29 C30 C31 120.8(9) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C30 C31 C32 120.1(9) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? N4 C32 C31 120.0(8) . . ? N4 C32 C33 116.2(8) . . ? C31 C32 C33 123.8(9) . . ? N5 C33 C34 121.0(8) . . ? N5 C33 C32 114.6(9) . . ? C34 C33 C32 124.4(9) . . ? C35 C34 C33 119.3(9) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C36 119.6(10) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C35 C36 C37 119.2(9) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? N5 C37 C36 122.0(9) . . ? N5 C37 C38 114.3(9) . . ? C36 C37 C38 123.6(9) . . ? N6 C38 C37 116.4(9) . . ? N6 C38 C39 125.1(9) . . ? C37 C38 C39 118.4(9) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C45 C40 C41 120.7(10) . . ? C45 C40 N6 121.1(8) . . ? C41 C40 N6 118.3(10) . . ? C42 C41 C40 118.5(11) . . ? C42 C41 C46 116.1(11) . . ? C40 C41 C46 125.1(11) . . ? C41 C42 C43 118.5(11) . . ? C41 C42 H42 120.7 . . ? C43 C42 H42 120.7 . . ? C44 C43 C42 120.6(12) . . ? C44 C43 C49 119.0(14) . . ? C42 C43 C49 120.4(14) . . ? C45 C44 C43 118.8(12) . . ? C45 C44 H44 120.6 . . ? C43 C44 H44 120.6 . . ? C40 C45 C44 122.8(10) . . ? C40 C45 C52 120.3(9) . . ? C44 C45 C52 117.0(10) . . ? C47 C46 C41 112.3(10) . . ? C47 C46 C48 118.4(11) . . ? C41 C46 C48 103.9(12) . . ? C47 C46 H46 107.2 . . ? C41 C46 H46 107.2 . . ? C48 C46 H46 107.2 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 C51 124(2) . . ? C50 C49 C43 117.4(17) . . ? C51 C49 C43 108.9(11) . . ? C50 C49 H49 100.3 . . ? C51 C49 H49 100.3 . . ? C43 C49 H49 100.3 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C45 C52 C53 114.2(9) . . ? C45 C52 C54 111.2(8) . . ? C53 C52 C54 109.0(8) . . ? C45 C52 H52 107.4 . . ? C53 C52 H52 107.4 . . ? C54 C52 H52 107.4 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N7 C55 C56 178.4(11) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N2A Co1A N1A 75.3(4) . . ? N2A Co1A N3A 76.5(4) . . ? N1A Co1A N3A 147.6(3) . . ? N2A Co1A Br1A 151.5(2) . . ? N1A Co1A Br1A 93.2(3) . . ? N3A Co1A Br1A 104.2(2) . . ? N2A Co1A Br2A 94.1(2) . . ? N1A Co1A Br2A 104.4(2) . . ? N3A Co1A Br2A 93.20(17) . . ? Br1A Co1A Br2A 114.09(7) . . ? N5A Co2A N7A 164.0(3) . . ? N5A Co2A O1 95.2(3) . . ? N7A Co2A O1 84.3(3) . . ? N5A Co2A N6A 73.9(3) . . ? N7A Co2A N6A 90.1(3) . . ? O1 Co2A N6A 89.3(2) . . ? N5A Co2A N4A 77.8(3) . . ? N7A Co2A N4A 117.9(3) . . ? O1 Co2A N4A 83.3(2) . . ? N6A Co2A N4A 150.0(3) . . ? N5A Co2A Br3A 90.4(2) . . ? N7A Co2A Br3A 93.0(2) . . ? O1 Co2A Br3A 168.48(15) . . ? N6A Co2A Br3A 101.9(2) . . ? N4A Co2A Br3A 88.1(2) . . ? C17A N1A C1A 117.4(12) . . ? C17A N1A Co1A 111.6(9) . . ? C1A N1A Co1A 130.9(8) . . ? C18A N2A C22A 119.2(11) . . ? C18A N2A Co1A 119.4(8) . . ? C22A N2A Co1A 119.8(10) . . ? C23A N3A C27A 119.8(9) . . ? C23A N3A Co1A 110.0(8) . . ? C27A N3A Co1A 129.6(7) . . ? C28A N4A C32A 119.2(8) . . ? C28A N4A Co2A 129.8(6) . . ? C32A N4A Co2A 110.9(6) . . ? C37A N5A C33A 121.8(9) . . ? C37A N5A Co2A 120.8(6) . . ? C33A N5A Co2A 117.1(7) . . ? C38A N6A C40A 123.4(8) . . ? C38A N6A Co2A 114.0(7) . . ? C40A N6A Co2A 122.4(6) . . ? C55A N7A Co2A 163.9(8) . . ? C2A C1A C6A 124.3(11) . . ? C2A C1A N1A 118.2(11) . . ? C6A C1A N1A 117.5(11) . . ? C1A C2A C3A 116.4(11) . . ? C1A C2A C10A 123.5(11) . . ? C3A C2A C10A 119.9(11) . . ? C2A C3A C4A 122.9(11) . . ? C2A C3A H3A 118.5 . . ? C4A C3A H3A 118.5 . . ? C5A C4A C3A 117.1(11) . . ? C5A C4A C13A 124.0(12) . . ? C3A C4A C13A 118.7(12) . . ? C6A C5A C4A 123.7(11) . . ? C6A C5A H5A 118.2 . . ? C4A C5A H5A 118.2 . . ? C5A C6A C1A 115.6(11) . . ? C5A C6A C7A 121.7(10) . . ? C1A C6A C7A 122.7(11) . . ? C6A C7A C8A 109.2(10) . . ? C6A C7A C9A 110.8(11) . . ? C8A C7A C9A 111.8(10) . . ? C6A C7A H7A 108.3 . . ? C8A C7A H7A 108.3 . . ? C9A C7A H7A 108.3 . . ? C7A C8A H8A1 109.5 . . ? C7A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C7A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C7A C9A H9A1 109.5 . . ? C7A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C7A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C11A C10A C2A 111.0(12) . . ? C11A C10A C12A 107.9(11) . . ? C2A C10A C12A 110.6(14) . . ? C11A C10A H10A 109.1 . . ? C2A C10A H10A 109.1 . . ? C12A C10A H10A 109.1 . . ? C10A C11A H11D 109.5 . . ? C10A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? C10A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? C10A C12A H12D 109.5 . . ? C10A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C10A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C14A C13A C15A 110.0(17) . . ? C14A C13A C4A 103.2(18) . . ? C15A C13A C4A 121.4(17) . . ? C14A C13A H13A 107.2 . . ? C15A C13A H13A 107.2 . . ? C4A C13A H13A 107.2 . . ? C13A C14A H14D 109.5 . . ? C13A C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C13A C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C13A C15A H15D 109.5 . . ? C13A C15A H15E 109.5 . . ? H15D C15A H15E 109.5 . . ? C13A C15A H15F 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? C17A C16A H16D 109.5 . . ? C17A C16A H16E 109.5 . . ? H16D C16A H16E 109.5 . . ? C17A C16A H16F 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? N1A C17A C18A 119.9(13) . . ? N1A C17A C16A 126.8(12) . . ? C18A C17A C16A 113.3(13) . . ? N2A C18A C19A 120.6(11) . . ? N2A C18A C17A 109.3(13) . . ? C19A C18A C17A 130.0(15) . . ? C20A C19A C18A 118.8(13) . . ? C20A C19A H19A 120.6 . . ? C18A C19A H19A 120.6 . . ? C19A C20A C21A 121.5(14) . . ? C19A C20A H20A 119.2 . . ? C21A C20A H20A 119.2 . . ? C20A C21A C22A 117.0(14) . . ? C20A C21A H21A 121.5 . . ? C22A C21A H21A 121.5 . . ? N2A C22A C21A 122.8(13) . . ? N2A C22A C23A 111.6(12) . . ? C21A C22A C23A 125.6(13) . . ? N3A C23A C24A 121.6(11) . . ? N3A C23A C22A 120.1(10) . . ? C24A C23A C22A 118.3(11) . . ? C25A C24A C23A 117.5(11) . . ? C25A C24A H24A 121.3 . . ? C23A C24A H24A 121.3 . . ? C24A C25A C26A 120.8(10) . . ? C24A C25A H25A 119.6 . . ? C26A C25A H25A 119.6 . . ? C27A C26A C25A 117.9(11) . . ? C27A C26A H26A 121.0 . . ? C25A C26A H26A 121.0 . . ? N3A C27A C26A 122.2(10) . . ? N3A C27A C28A 119.3(9) . . ? C26A C27A C28A 117.7(11) . . ? N4A C28A C29A 120.6(9) . . ? N4A C28A C27A 118.6(8) . . ? C29A C28A C27A 120.6(10) . . ? C28A C29A C30A 118.6(10) . . ? C28A C29A H29A 120.7 . . ? C30A C29A H29A 120.7 . . ? C31A C30A C29A 120.3(9) . . ? C31A C30A H30A 119.8 . . ? C29A C30A H30A 119.8 . . ? C32A C31A C30A 117.8(10) . . ? C32A C31A H31A 121.1 . . ? C30A C31A H31A 121.1 . . ? C31A C32A N4A 123.2(10) . . ? C31A C32A C33A 120.4(10) . . ? N4A C32A C33A 116.4(8) . . ? N5A C33A C34A 115.0(10) . . ? N5A C33A C32A 116.5(9) . . ? C34A C33A C32A 128.5(10) . . ? C35A C34A C33A 121.5(10) . . ? C35A C34A H34A 119.3 . . ? C33A C34A H34A 119.3 . . ? C36A C35A C34A 119.5(11) . . ? C36A C35A H35A 120.3 . . ? C34A C35A H35A 120.3 . . ? C37A C36A C35A 118.1(11) . . ? C37A C36A H36A 120.9 . . ? C35A C36A H36A 120.9 . . ? N5A C37A C36A 124.0(10) . . ? N5A C37A C38A 113.8(9) . . ? C36A C37A C38A 122.2(11) . . ? N6A C38A C39A 125.7(9) . . ? N6A C38A C37A 116.9(10) . . ? C39A C38A C37A 117.4(9) . . ? C38A C39A H39D 109.5 . . ? C38A C39A H39E 109.5 . . ? H39D C39A H39E 109.5 . . ? C38A C39A H39F 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C41A C40A C45A 119.4(9) . . ? C41A C40A N6A 122.3(9) . . ? C45A C40A N6A 118.2(10) . . ? C42A C41A C40A 117.6(9) . . ? C42A C41A C46A 119.9(11) . . ? C40A C41A C46A 122.5(10) . . ? C43A C42A C41A 124.0(10) . . ? C43A C42A H42A 118.0 . . ? C41A C42A H42A 118.0 . . ? C42A C43A C44A 119.8(10) . . ? C42A C43A C49A 121.6(11) . . ? C44A C43A C49A 118.6(10) . . ? C43A C44A C45A 118.7(9) . . ? C43A C44A H44A 120.6 . . ? C45A C44A H44A 120.6 . . ? C44A C45A C40A 120.0(10) . . ? C44A C45A C52A 120.0(9) . . ? C40A C45A C52A 119.9(9) . . ? C41A C46A C47A 110.4(8) . . ? C41A C46A C48A 112.5(9) . . ? C47A C46A C48A 109.7(9) . . ? C41A C46A H46A 108.0 . . ? C47A C46A H46A 108.0 . . ? C48A C46A H46A 108.0 . . ? C46A C47A H47D 109.5 . . ? C46A C47A H47E 109.5 . . ? H47D C47A H47E 109.5 . . ? C46A C47A H47F 109.5 . . ? H47D C47A H47F 109.5 . . ? H47E C47A H47F 109.5 . . ? C46A C48A H48D 109.5 . . ? C46A C48A H48E 109.5 . . ? H48D C48A H48E 109.5 . . ? C46A C48A H48F 109.5 . . ? H48D C48A H48F 109.5 . . ? H48E C48A H48F 109.5 . . ? C50A C49A C51A 117.1(11) . . ? C50A C49A C43A 113.4(11) . . ? C51A C49A C43A 108.5(11) . . ? C50A C49A H49A 105.6 . . ? C51A C49A H49A 105.6 . . ? C43A C49A H49A 105.6 . . ? C49A C50A H50G 109.5 . . ? C49A C50A H50H 109.5 . . ? H50G C50A H50H 109.5 . . ? C49A C50A H50I 109.5 . . ? H50G C50A H50I 109.5 . . ? H50H C50A H50I 109.5 . . ? C49A C51A H51D 109.5 . . ? C49A C51A H51E 109.5 . . ? H51D C51A H51E 109.5 . . ? C49A C51A H51F 109.5 . . ? H51D C51A H51F 109.5 . . ? H51E C51A H51F 109.5 . . ? C45A C52A C53A 112.5(9) . . ? C45A C52A C54A 111.1(9) . . ? C53A C52A C54A 111.7(9) . . ? C45A C52A H52A 107.0 . . ? C53A C52A H52A 107.0 . . ? C54A C52A H52A 107.0 . . ? C52A C53A H53D 109.5 . . ? C52A C53A H53E 109.5 . . ? H53D C53A H53E 109.5 . . ? C52A C53A H53F 109.5 . . ? H53D C53A H53F 109.5 . . ? H53E C53A H53F 109.5 . . ? C52A C54A H54D 109.5 . . ? C52A C54A H54E 109.5 . . ? H54D C54A H54E 109.5 . . ? C52A C54A H54F 109.5 . . ? H54D C54A H54F 109.5 . . ? H54E C54A H54F 109.5 . . ? N7A C55A C56A 179.4(14) . . ? C55A C56A H56D 109.5 . . ? C55A C56A H56E 109.5 . . ? H56D C56A H56E 109.5 . . ? C55A C56A H56F 109.5 . . ? H56D C56A H56F 109.5 . . ? H56E C56A H56F 109.5 . . ? Br5 Co3 Br6 105.69(6) . . ? Br5 Co3 Br7 105.57(6) . . ? Br6 Co3 Br7 113.84(6) . . ? Br5 Co3 Br4 115.54(6) . . ? Br6 Co3 Br4 106.88(6) . . ? Br7 Co3 Br4 109.50(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Co2 Br2 Co1 -79.9(2) . . . . ? N6 Co2 Br2 Co1 -155.2(2) . . . . ? N4 Co2 Br2 Co1 -1.9(2) . . . . ? Br3 Co2 Br2 Co1 97.02(7) . . . . ? N2 Co1 Br2 Co2 -137.1(2) . . . . ? N7 Co1 Br2 Co2 61.6(2) . . . . ? N3 Co1 Br2 Co2 -60.28(17) . . . . ? N1 Co1 Br2 Co2 147.8(2) . . . . ? Br1 Co1 Br2 Co2 -33.8(3) . . . . ? N2 Co1 N1 C17 -2.9(5) . . . . ? N7 Co1 N1 C17 169.7(6) . . . . ? N3 Co1 N1 C17 5.6(8) . . . . ? Br1 Co1 N1 C17 -100.7(5) . . . . ? Br2 Co1 N1 C17 78.9(5) . . . . ? N2 Co1 N1 C1 177.8(7) . . . . ? N7 Co1 N1 C1 -9.6(7) . . . . ? N3 Co1 N1 C1 -173.7(6) . . . . ? Br1 Co1 N1 C1 80.0(7) . . . . ? Br2 Co1 N1 C1 -100.3(7) . . . . ? N7 Co1 N2 C22 154.1(8) . . . . ? N3 Co1 N2 C22 0.7(5) . . . . ? N1 Co1 N2 C22 176.4(6) . . . . ? Br1 Co1 N2 C22 -85.6(5) . . . . ? Br2 Co1 N2 C22 82.4(5) . . . . ? N7 Co1 N2 C18 -19.5(11) . . . . ? N3 Co1 N2 C18 -172.9(6) . . . . ? N1 Co1 N2 C18 2.8(5) . . . . ? Br1 Co1 N2 C18 100.8(5) . . . . ? Br2 Co1 N2 C18 -91.2(5) . . . . ? N2 Co1 N3 C23 -5.7(5) . . . . ? N7 Co1 N3 C23 -175.5(5) . . . . ? N1 Co1 N3 C23 -14.3(7) . . . . ? Br1 Co1 N3 C23 94.9(5) . . . . ? Br2 Co1 N3 C23 -90.5(5) . . . . ? N2 Co1 N3 C27 -175.1(6) . . . . ? N7 Co1 N3 C27 15.1(7) . . . . ? N1 Co1 N3 C27 176.4(5) . . . . ? Br1 Co1 N3 C27 -74.5(6) . . . . ? Br2 Co1 N3 C27 100.1(6) . . . . ? N5 Co2 N4 C28 -174.5(7) . . . . ? N6 Co2 N4 C28 -167.2(6) . . . . ? Br3 Co2 N4 C28 -42.0(6) . . . . ? Br2 Co2 N4 C28 77.4(6) . . . . ? N5 Co2 N4 C32 -10.3(5) . . . . ? N6 Co2 N4 C32 -2.9(8) . . . . ? Br3 Co2 N4 C32 122.3(5) . . . . ? Br2 Co2 N4 C32 -118.3(5) . . . . ? N6 Co2 N5 C37 11.3(6) . . . . ? N4 Co2 N5 C37 -172.5(6) . . . . ? Br3 Co2 N5 C37 105.2(6) . . . . ? Br2 Co2 N5 C37 -78.5(6) . . . . ? N6 Co2 N5 C33 -173.4(6) . . . . ? N4 Co2 N5 C33 2.8(5) . . . . ? Br3 Co2 N5 C33 -79.5(6) . . . . ? Br2 Co2 N5 C33 96.9(5) . . . . ? N5 Co2 N6 C38 -11.9(6) . . . . ? N4 Co2 N6 C38 -19.3(8) . . . . ? Br3 Co2 N6 C38 -142.4(5) . . . . ? Br2 Co2 N6 C38 97.0(6) . . . . ? N5 Co2 N6 C40 166.5(7) . . . . ? N4 Co2 N6 C40 159.1(7) . . . . ? Br3 Co2 N6 C40 36.0(7) . . . . ? Br2 Co2 N6 C40 -84.6(7) . . . . ? N2 Co1 N7 C55 49(3) . . . . ? N3 Co1 N7 C55 -162(2) . . . . ? N1 Co1 N7 C55 27(2) . . . . ? Br1 Co1 N7 C55 -73(2) . . . . ? Br2 Co1 N7 C55 119(2) . . . . ? C17 N1 C1 C6 92.5(10) . . . . ? Co1 N1 C1 C6 -88.3(9) . . . . ? C17 N1 C1 C2 -89.5(10) . . . . ? Co1 N1 C1 C2 89.7(9) . . . . ? C6 C1 C2 C3 1.5(13) . . . . ? N1 C1 C2 C3 -176.5(8) . . . . ? C6 C1 C2 C10 -177.5(8) . . . . ? N1 C1 C2 C10 4.5(12) . . . . ? C1 C2 C3 C4 -0.1(16) . . . . ? C10 C2 C3 C4 178.9(10) . . . . ? C2 C3 C4 C5 -0.7(17) . . . . ? C2 C3 C4 C13 178.6(10) . . . . ? C3 C4 C5 C6 0.0(17) . . . . ? C13 C4 C5 C6 -179.2(10) . . . . ? C2 C1 C6 C5 -2.1(13) . . . . ? N1 C1 C6 C5 175.9(7) . . . . ? C2 C1 C6 C7 177.2(8) . . . . ? N1 C1 C6 C7 -4.8(13) . . . . ? C4 C5 C6 C1 1.4(15) . . . . ? C4 C5 C6 C7 -177.9(10) . . . . ? C1 C6 C7 C9 133.1(9) . . . . ? C5 C6 C7 C9 -47.6(12) . . . . ? C1 C6 C7 C8 -104.4(10) . . . . ? C5 C6 C7 C8 74.9(11) . . . . ? C3 C2 C10 C12 56.5(12) . . . . ? C1 C2 C10 C12 -124.5(9) . . . . ? C3 C2 C10 C11 -61.2(12) . . . . ? C1 C2 C10 C11 117.8(10) . . . . ? C3 C4 C13 C14 168.6(12) . . . . ? C5 C4 C13 C14 -12.2(19) . . . . ? C3 C4 C13 C15 -61.0(16) . . . . ? C5 C4 C13 C15 118.2(14) . . . . ? C1 N1 C17 C18 -177.9(7) . . . . ? Co1 N1 C17 C18 2.7(9) . . . . ? C1 N1 C17 C16 0.4(12) . . . . ? Co1 N1 C17 C16 -178.9(6) . . . . ? C22 N2 C18 C19 2.3(11) . . . . ? Co1 N2 C18 C19 175.7(5) . . . . ? C22 N2 C18 C17 -175.9(7) . . . . ? Co1 N2 C18 C17 -2.4(9) . . . . ? N1 C17 C18 N2 -0.5(11) . . . . ? C16 C17 C18 N2 -179.0(7) . . . . ? N1 C17 C18 C19 -178.5(8) . . . . ? C16 C17 C18 C19 3.0(12) . . . . ? N2 C18 C19 C20 -1.7(12) . . . . ? C17 C18 C19 C20 176.3(8) . . . . ? C18 C19 C20 C21 0.2(13) . . . . ? C19 C20 C21 C22 0.8(12) . . . . ? C18 N2 C22 C21 -1.3(11) . . . . ? Co1 N2 C22 C21 -174.7(5) . . . . ? C18 N2 C22 C23 177.5(6) . . . . ? Co1 N2 C22 C23 4.1(9) . . . . ? C20 C21 C22 N2 -0.3(11) . . . . ? C20 C21 C22 C23 -178.9(7) . . . . ? C27 N3 C23 C24 1.3(11) . . . . ? Co1 N3 C23 C24 -169.1(6) . . . . ? C27 N3 C23 C22 179.7(6) . . . . ? Co1 N3 C23 C22 9.3(8) . . . . ? N2 C22 C23 N3 -9.2(9) . . . . ? C21 C22 C23 N3 169.6(7) . . . . ? N2 C22 C23 C24 169.2(7) . . . . ? C21 C22 C23 C24 -12.0(12) . . . . ? N3 C23 C24 C25 -1.1(12) . . . . ? C22 C23 C24 C25 -179.5(7) . . . . ? C23 C24 C25 C26 1.3(11) . . . . ? C24 C25 C26 C27 -1.8(12) . . . . ? C23 N3 C27 C26 -1.7(10) . . . . ? Co1 N3 C27 C26 167.1(5) . . . . ? C23 N3 C27 C28 179.6(7) . . . . ? Co1 N3 C27 C28 -11.6(9) . . . . ? C25 C26 C27 N3 2.0(12) . . . . ? C25 C26 C27 C28 -179.3(8) . . . . ? C32 N4 C28 C29 -5.2(12) . . . . ? Co2 N4 C28 C29 158.1(6) . . . . ? C32 N4 C28 C27 173.9(7) . . . . ? Co2 N4 C28 C27 -22.8(10) . . . . ? N3 C27 C28 N4 -54.2(10) . . . . ? C26 C27 C28 N4 127.1(8) . . . . ? N3 C27 C28 C29 125.1(8) . . . . ? C26 C27 C28 C29 -53.6(11) . . . . ? N4 C28 C29 C30 2.2(13) . . . . ? C27 C28 C29 C30 -177.0(8) . . . . ? C28 C29 C30 C31 3.0(13) . . . . ? C29 C30 C31 C32 -5.0(14) . . . . ? C28 N4 C32 C31 3.0(11) . . . . ? Co2 N4 C32 C31 -163.4(6) . . . . ? C28 N4 C32 C33 -177.8(7) . . . . ? Co2 N4 C32 C33 15.9(8) . . . . ? C30 C31 C32 N4 2.0(12) . . . . ? C30 C31 C32 C33 -177.2(8) . . . . ? C37 N5 C33 C34 1.3(11) . . . . ? Co2 N5 C33 C34 -174.1(6) . . . . ? C37 N5 C33 C32 -180.0(7) . . . . ? Co2 N5 C33 C32 4.6(9) . . . . ? N4 C32 C33 N5 -14.4(10) . . . . ? C31 C32 C33 N5 164.8(7) . . . . ? N4 C32 C33 C34 164.3(8) . . . . ? C31 C32 C33 C34 -16.5(13) . . . . ? N5 C33 C34 C35 -0.5(13) . . . . ? C32 C33 C34 C35 -179.1(8) . . . . ? C33 C34 C35 C36 0.3(13) . . . . ? C34 C35 C36 C37 -0.8(13) . . . . ? C33 N5 C37 C36 -1.9(11) . . . . ? Co2 N5 C37 C36 173.6(6) . . . . ? C33 N5 C37 C38 175.3(6) . . . . ? Co2 N5 C37 C38 -9.3(9) . . . . ? C35 C36 C37 N5 1.6(12) . . . . ? C35 C36 C37 C38 -175.3(7) . . . . ? C40 N6 C38 C37 -167.5(7) . . . . ? Co2 N6 C38 C37 11.1(9) . . . . ? C40 N6 C38 C39 7.2(12) . . . . ? Co2 N6 C38 C39 -174.2(6) . . . . ? N5 C37 C38 N6 -2.4(10) . . . . ? C36 C37 C38 N6 174.7(8) . . . . ? N5 C37 C38 C39 -177.5(7) . . . . ? C36 C37 C38 C39 -0.4(12) . . . . ? C38 N6 C40 C45 93.3(11) . . . . ? Co2 N6 C40 C45 -85.1(10) . . . . ? C38 N6 C40 C41 -84.7(10) . . . . ? Co2 N6 C40 C41 97.0(10) . . . . ? C45 C40 C41 C42 -3.3(16) . . . . ? N6 C40 C41 C42 174.7(9) . . . . ? C45 C40 C41 C46 -177.4(11) . . . . ? N6 C40 C41 C46 0.6(16) . . . . ? C40 C41 C42 C43 1.7(18) . . . . ? C46 C41 C42 C43 176.4(11) . . . . ? C41 C42 C43 C44 1.2(19) . . . . ? C41 C42 C43 C49 -179.7(11) . . . . ? C42 C43 C44 C45 -2.6(18) . . . . ? C49 C43 C44 C45 178.2(11) . . . . ? C41 C40 C45 C44 1.8(16) . . . . ? N6 C40 C45 C44 -176.1(9) . . . . ? C41 C40 C45 C52 -179.5(9) . . . . ? N6 C40 C45 C52 2.6(14) . . . . ? C43 C44 C45 C40 1.1(16) . . . . ? C43 C44 C45 C52 -177.6(9) . . . . ? C42 C41 C46 C47 -59.0(15) . . . . ? C40 C41 C46 C47 115.2(13) . . . . ? C42 C41 C46 C48 70.2(13) . . . . ? C40 C41 C46 C48 -115.5(11) . . . . ? C44 C43 C49 C50 77(3) . . . . ? C42 C43 C49 C50 -102(3) . . . . ? C44 C43 C49 C51 -70.5(19) . . . . ? C42 C43 C49 C51 110.4(16) . . . . ? C40 C45 C52 C53 138.5(9) . . . . ? C44 C45 C52 C53 -42.8(12) . . . . ? C40 C45 C52 C54 -97.7(10) . . . . ? C44 C45 C52 C54 81.0(11) . . . . ? Co1 N7 C55 C56 -158(45) . . . . ? N2A Co1A N1A C17A -13.8(7) . . . . ? N3A Co1A N1A C17A -44.1(10) . . . . ? Br1A Co1A N1A C17A -167.4(7) . . . . ? Br2A Co1A N1A C17A 76.7(7) . . . . ? N2A Co1A N1A C1A 162.0(10) . . . . ? N3A Co1A N1A C1A 131.7(9) . . . . ? Br1A Co1A N1A C1A 8.4(9) . . . . ? Br2A Co1A N1A C1A -107.5(9) . . . . ? N1A Co1A N2A C18A 20.2(8) . . . . ? N3A Co1A N2A C18A -175.9(8) . . . . ? Br1A Co1A N2A C18A 89.1(9) . . . . ? Br2A Co1A N2A C18A -83.6(8) . . . . ? N1A Co1A N2A C22A -174.6(8) . . . . ? N3A Co1A N2A C22A -10.7(7) . . . . ? Br1A Co1A N2A C22A -105.7(9) . . . . ? Br2A Co1A N2A C22A 81.6(7) . . . . ? N2A Co1A N3A C23A 2.0(5) . . . . ? N1A Co1A N3A C23A 32.1(9) . . . . ? Br1A Co1A N3A C23A 152.7(5) . . . . ? Br2A Co1A N3A C23A -91.5(5) . . . . ? N2A Co1A N3A C27A -169.1(8) . . . . ? N1A Co1A N3A C27A -139.0(8) . . . . ? Br1A Co1A N3A C27A -18.5(7) . . . . ? Br2A Co1A N3A C27A 97.4(7) . . . . ? N5A Co2A N4A C28A -172.9(9) . . . . ? N7A Co2A N4A C28A 3.9(10) . . . . ? O1 Co2A N4A C28A -76.1(9) . . . . ? N6A Co2A N4A C28A -152.9(8) . . . . ? Br3A Co2A N4A C28A 96.3(9) . . . . ? N5A Co2A N4A C32A 10.0(6) . . . . ? N7A Co2A N4A C32A -173.2(6) . . . . ? O1 Co2A N4A C32A 106.9(6) . . . . ? N6A Co2A N4A C32A 30.1(10) . . . . ? Br3A Co2A N4A C32A -80.8(6) . . . . ? N7A Co2A N5A C37A 6.9(17) . . . . ? O1 Co2A N5A C37A 94.6(8) . . . . ? N6A Co2A N5A C37A 6.8(8) . . . . ? N4A Co2A N5A C37A 176.5(9) . . . . ? Br3A Co2A N5A C37A -95.5(8) . . . . ? N7A Co2A N5A C33A -178.9(10) . . . . ? O1 Co2A N5A C33A -91.2(7) . . . . ? N6A Co2A N5A C33A -179.0(7) . . . . ? N4A Co2A N5A C33A -9.2(7) . . . . ? Br3A Co2A N5A C33A 78.7(7) . . . . ? N5A Co2A N6A C38A -4.3(7) . . . . ? N7A Co2A N6A C38A 175.7(8) . . . . ? O1 Co2A N6A C38A -100.0(7) . . . . ? N4A Co2A N6A C38A -24.7(11) . . . . ? Br3A Co2A N6A C38A 82.6(7) . . . . ? N5A Co2A N6A C40A 170.8(8) . . . . ? N7A Co2A N6A C40A -9.2(7) . . . . ? O1 Co2A N6A C40A 75.2(7) . . . . ? N4A Co2A N6A C40A 150.4(7) . . . . ? Br3A Co2A N6A C40A -102.3(7) . . . . ? N5A Co2A N7A C55A 8(4) . . . . ? O1 Co2A N7A C55A -81(4) . . . . ? N6A Co2A N7A C55A 8(4) . . . . ? N4A Co2A N7A C55A -160(4) . . . . ? Br3A Co2A N7A C55A 110(4) . . . . ? C17A N1A C1A C2A 74.0(15) . . . . ? Co1A N1A C1A C2A -101.6(13) . . . . ? C17A N1A C1A C6A -106.6(13) . . . . ? Co1A N1A C1A C6A 77.9(13) . . . . ? C6A C1A C2A C3A -1(2) . . . . ? N1A C1A C2A C3A 178.1(12) . . . . ? C6A C1A C2A C10A -176.6(13) . . . . ? N1A C1A C2A C10A 3(2) . . . . ? C1A C2A C3A C4A -1(2) . . . . ? C10A C2A C3A C4A 174.9(14) . . . . ? C2A C3A C4A C5A 3(2) . . . . ? C2A C3A C4A C13A -172.2(16) . . . . ? C3A C4A C5A C6A -3(2) . . . . ? C13A C4A C5A C6A 171.4(16) . . . . ? C4A C5A C6A C1A 1(2) . . . . ? C4A C5A C6A C7A 179.7(13) . . . . ? C2A C1A C6A C5A 1(2) . . . . ? N1A C1A C6A C5A -178.5(11) . . . . ? C2A C1A C6A C7A -177.4(13) . . . . ? N1A C1A C6A C7A 3.1(19) . . . . ? C5A C6A C7A C8A -81.3(16) . . . . ? C1A C6A C7A C8A 96.9(14) . . . . ? C5A C6A C7A C9A 42.3(17) . . . . ? C1A C6A C7A C9A -139.4(12) . . . . ? C1A C2A C10A C11A 111.1(15) . . . . ? C3A C2A C10A C11A -64(2) . . . . ? C1A C2A C10A C12A -129.1(15) . . . . ? C3A C2A C10A C12A 55.7(18) . . . . ? C5A C4A C13A C14A 116.6(15) . . . . ? C3A C4A C13A C14A -69(2) . . . . ? C5A C4A C13A C15A -119.8(19) . . . . ? C3A C4A C13A C15A 55(2) . . . . ? C1A N1A C17A C18A -169.1(9) . . . . ? Co1A N1A C17A C18A 7.3(12) . . . . ? C1A N1A C17A C16A 11.6(16) . . . . ? Co1A N1A C17A C16A -172.0(8) . . . . ? C22A N2A C18A C19A -4.5(15) . . . . ? Co1A N2A C18A C19A 160.8(8) . . . . ? C22A N2A C18A C17A 173.0(8) . . . . ? Co1A N2A C18A C17A -21.7(11) . . . . ? N1A C17A C18A N2A 8.2(14) . . . . ? C16A C17A C18A N2A -172.5(8) . . . . ? N1A C17A C18A C19A -174.6(11) . . . . ? C16A C17A C18A C19A 4.7(16) . . . . ? N2A C18A C19A C20A 1.9(17) . . . . ? C17A C18A C19A C20A -175.0(11) . . . . ? C18A C19A C20A C21A 0.8(19) . . . . ? C19A C20A C21A C22A -0.8(19) . . . . ? C18A N2A C22A C21A 4.6(15) . . . . ? Co1A N2A C22A C21A -160.7(8) . . . . ? C18A N2A C22A C23A -178.2(8) . . . . ? Co1A N2A C22A C23A 16.5(10) . . . . ? C20A C21A C22A N2A -1.9(17) . . . . ? C20A C21A C22A C23A -178.7(10) . . . . ? C27A N3A C23A C24A -1.7(13) . . . . ? Co1A N3A C23A C24A -173.9(7) . . . . ? C27A N3A C23A C22A 178.2(8) . . . . ? Co1A N3A C23A C22A 6.1(10) . . . . ? N2A C22A C23A N3A -14.6(12) . . . . ? C21A C22A C23A N3A 162.5(10) . . . . ? N2A C22A C23A C24A 165.4(8) . . . . ? C21A C22A C23A C24A -17.6(15) . . . . ? N3A C23A C24A C25A 3.3(14) . . . . ? C22A C23A C24A C25A -176.6(9) . . . . ? C23A C24A C25A C26A -4.5(15) . . . . ? C24A C25A C26A C27A 4.0(14) . . . . ? C23A N3A C27A C26A 1.2(13) . . . . ? Co1A N3A C27A C26A 171.6(6) . . . . ? C23A N3A C27A C28A 171.5(8) . . . . ? Co1A N3A C27A C28A -18.1(12) . . . . ? C25A C26A C27A N3A -2.4(13) . . . . ? C25A C26A C27A C28A -172.8(8) . . . . ? C32A N4A C28A C29A 0.6(15) . . . . ? Co2A N4A C28A C29A -176.3(7) . . . . ? C32A N4A C28A C27A 176.1(9) . . . . ? Co2A N4A C28A C27A -0.8(14) . . . . ? N3A C27A C28A N4A 124.4(10) . . . . ? C26A C27A C28A N4A -64.9(12) . . . . ? N3A C27A C28A C29A -60.1(13) . . . . ? C26A C27A C28A C29A 110.6(11) . . . . ? N4A C28A C29A C30A 3.9(15) . . . . ? C27A C28A C29A C30A -171.5(10) . . . . ? C28A C29A C30A C31A -5.0(16) . . . . ? C29A C30A C31A C32A 1.5(16) . . . . ? C30A C31A C32A N4A 3.3(16) . . . . ? C30A C31A C32A C33A -174.2(9) . . . . ? C28A N4A C32A C31A -4.4(15) . . . . ? Co2A N4A C32A C31A 173.0(8) . . . . ? C28A N4A C32A C33A 173.2(9) . . . . ? Co2A N4A C32A C33A -9.4(10) . . . . ? C37A N5A C33A C34A 1.7(14) . . . . ? Co2A N5A C33A C34A -172.5(7) . . . . ? C37A N5A C33A C32A -178.6(9) . . . . ? Co2A N5A C33A C32A 7.3(11) . . . . ? C31A C32A C33A N5A 179.9(9) . . . . ? N4A C32A C33A N5A 2.3(13) . . . . ? C31A C32A C33A C34A -0.4(16) . . . . ? N4A C32A C33A C34A -178.0(9) . . . . ? N5A C33A C34A C35A 0.8(16) . . . . ? C32A C33A C34A C35A -178.9(11) . . . . ? C33A C34A C35A C36A -1.6(19) . . . . ? C34A C35A C36A C37A 0.0(19) . . . . ? C33A N5A C37A C36A -3.5(17) . . . . ? Co2A N5A C37A C36A 170.5(9) . . . . ? C33A N5A C37A C38A 178.0(9) . . . . ? Co2A N5A C37A C38A -8.1(13) . . . . ? C35A C36A C37A N5A 2.6(19) . . . . ? C35A C36A C37A C38A -179.0(11) . . . . ? C40A N6A C38A C39A 6.3(17) . . . . ? Co2A N6A C38A C39A -178.7(8) . . . . ? C40A N6A C38A C37A -173.3(9) . . . . ? Co2A N6A C38A C37A 1.7(12) . . . . ? N5A C37A C38A N6A 3.7(15) . . . . ? C36A C37A C38A N6A -174.9(10) . . . . ? N5A C37A C38A C39A -175.9(9) . . . . ? C36A C37A C38A C39A 5.5(16) . . . . ? C38A N6A C40A C41A 78.7(14) . . . . ? Co2A N6A C40A C41A -96.0(10) . . . . ? C38A N6A C40A C45A -104.4(11) . . . . ? Co2A N6A C40A C45A 80.9(10) . . . . ? C45A C40A C41A C42A -3.7(15) . . . . ? N6A C40A C41A C42A 173.1(9) . . . . ? C45A C40A C41A C46A 174.7(9) . . . . ? N6A C40A C41A C46A -8.4(16) . . . . ? C40A C41A C42A C43A -0.9(17) . . . . ? C46A C41A C42A C43A -179.3(11) . . . . ? C41A C42A C43A C44A 5.6(18) . . . . ? C41A C42A C43A C49A -175.0(11) . . . . ? C42A C43A C44A C45A -5.5(16) . . . . ? C49A C43A C44A C45A 175.1(10) . . . . ? C43A C44A C45A C40A 1.0(15) . . . . ? C43A C44A C45A C52A 178.6(10) . . . . ? C41A C40A C45A C44A 3.6(15) . . . . ? N6A C40A C45A C44A -173.4(9) . . . . ? C41A C40A C45A C52A -174.0(10) . . . . ? N6A C40A C45A C52A 9.0(14) . . . . ? C42A C41A C46A C47A 67.6(14) . . . . ? C40A C41A C46A C47A -110.8(12) . . . . ? C42A C41A C46A C48A -55.3(13) . . . . ? C40A C41A C46A C48A 126.3(11) . . . . ? C42A C43A C49A C50A 40.2(17) . . . . ? C44A C43A C49A C50A -140.5(11) . . . . ? C42A C43A C49A C51A -91.8(14) . . . . ? C44A C43A C49A C51A 87.6(13) . . . . ? C44A C45A C52A C53A 44.8(14) . . . . ? C40A C45A C52A C53A -137.6(9) . . . . ? C44A C45A C52A C54A -81.3(11) . . . . ? C40A C45A C52A C54A 96.3(10) . . . . ? Co2A N7A C55A C56A -58(100) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.002 _refine_diff_density_min -0.670 _refine_diff_density_rms 0.105 # Attachment '09039.cif' data_09039 _database_code_depnum_ccdc_archive 'CCDC 733358' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' (C114 H137 Cl6 N15 Ni4) (Ni Cl4)45(C H3 C N)' _chemical_formula_sum 'C204 H272 Cl10 N60 Ni5' _chemical_formula_weight 4212.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.953(8) _cell_length_b 30.086(13) _cell_length_c 30.593(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.776(9) _cell_angle_gamma 90.00 _cell_volume 15525(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 700 _cell_measurement_theta_min 2.432 _cell_measurement_theta_max 27.052 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8904 _exptl_absorpt_coefficient_mu 0.859 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7767 _exptl_absorpt_correction_T_max 0.8749 _exptl_absorpt_process_details ; absorption correction based on 5853 reflections(SADABS);Rint 0.2015 before correction and 0.0713 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 120386 _diffrn_reflns_av_R_equivalents 0.2767 _diffrn_reflns_av_sigmaI/netI 0.3929 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 0.95 _diffrn_reflns_theta_max 26.00 _reflns_number_total 30466 _reflns_number_gt 6951 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1180P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 30466 _refine_ls_number_parameters 681 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2926 _refine_ls_R_factor_gt 0.1210 _refine_ls_wR_factor_ref 0.3430 _refine_ls_wR_factor_gt 0.2877 _refine_ls_goodness_of_fit_ref 0.847 _refine_ls_restrained_S_all 0.847 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.51971(9) 0.06819(5) 0.58719(5) 0.0202(4) Uani 1 1 d . . . Ni2 Ni 0.74351(9) 0.06673(5) 0.62887(5) 0.0214(4) Uani 1 1 d . . . Cl1 Cl 0.62512(18) 0.11115(10) 0.61238(11) 0.0316(9) Uani 1 1 d . . . Cl2 Cl 0.44708(19) 0.02148(11) 0.62211(11) 0.0325(8) Uani 1 1 d . . . Cl3 Cl 0.8443(2) 0.01417(10) 0.64192(11) 0.0304(8) Uani 1 1 d . . . N1 N 0.4435(5) 0.1264(3) 0.5854(3) 0.018(2) Uiso 1 1 d . . . N2 N 0.5152(6) 0.0864(3) 0.5262(4) 0.033(3) Uiso 1 1 d . . . N3 N 0.5933(6) 0.0189(3) 0.5622(4) 0.030(3) Uiso 1 1 d . . . N4 N 0.6651(6) 0.0174(3) 0.6518(3) 0.022(2) Uiso 1 1 d . . . N5 N 0.7362(5) 0.0816(3) 0.6880(3) 0.009(2) Uiso 1 1 d . . . N6 N 0.8130(6) 0.1293(3) 0.6334(3) 0.023(3) Uiso 1 1 d . . . N7 N 0.7571(6) 0.0618(3) 0.5641(4) 0.034(3) Uiso 1 1 d . . . C1 C 0.4038(8) 0.1426(4) 0.6197(4) 0.030(3) Uiso 1 1 d . . . C2 C 0.4384(8) 0.1740(4) 0.6499(4) 0.030(3) Uiso 1 1 d . . . C3 C 0.4014(8) 0.1865(4) 0.6878(5) 0.039(4) Uiso 1 1 d . . . H3 H 0.4285 0.2058 0.7088 0.047 Uiso 1 1 calc R . . C4 C 0.3253(8) 0.1707(4) 0.6947(5) 0.036(4) Uiso 1 1 d . . . C5 C 0.2943(8) 0.1381(4) 0.6646(4) 0.033(4) Uiso 1 1 d . . . H5 H 0.2466 0.1236 0.6704 0.040 Uiso 1 1 calc R . . C6 C 0.3290(7) 0.1259(4) 0.6271(4) 0.023(3) Uiso 1 1 d . . . C7 C 0.4394(6) 0.1462(3) 0.5491(3) 0.009(2) Uiso 1 1 d . . . C8 C 0.3992(8) 0.1898(4) 0.5381(4) 0.035(4) Uiso 1 1 d . . . H8A H 0.3659 0.1978 0.5612 0.052 Uiso 1 1 calc R . . H8B H 0.3661 0.1872 0.5100 0.052 Uiso 1 1 calc R . . H8C H 0.4393 0.2129 0.5357 0.052 Uiso 1 1 calc R . . C9 C 0.4802(7) 0.1277(4) 0.5140(4) 0.026(3) Uiso 1 1 d . . . C10 C 0.4844(7) 0.1407(4) 0.4711(4) 0.030(3) Uiso 1 1 d . . . H10 H 0.4582 0.1675 0.4617 0.036 Uiso 1 1 calc R . . C11 C 0.5231(8) 0.1181(4) 0.4411(5) 0.043(4) Uiso 1 1 d . . . H11 H 0.5255 0.1299 0.4125 0.051 Uiso 1 1 calc R . . C12 C 0.5602(7) 0.0763(4) 0.4530(4) 0.024(3) Uiso 1 1 d . . . H12 H 0.5868 0.0592 0.4329 0.029 Uiso 1 1 calc R . . C13 C 0.5544(8) 0.0626(4) 0.4959(5) 0.034(4) Uiso 1 1 d . . . C14 C 0.5942(8) 0.0246(4) 0.5179(5) 0.032(3) Uiso 1 1 d . . . C15 C 0.6303(7) -0.0078(4) 0.4926(4) 0.032(3) Uiso 1 1 d . . . H15 H 0.6299 -0.0049 0.4616 0.039 Uiso 1 1 calc R . . C16 C 0.6669(7) -0.0446(4) 0.5153(4) 0.032(3) Uiso 1 1 d . . . H16 H 0.6928 -0.0667 0.4998 0.039 Uiso 1 1 calc R . . C17 C 0.6646(7) -0.0478(4) 0.5579(4) 0.030(3) Uiso 1 1 d . . . H17 H 0.6897 -0.0728 0.5722 0.036 Uiso 1 1 calc R . . C18 C 0.6297(8) -0.0187(4) 0.5828(5) 0.036(4) Uiso 1 1 d . . . C19 C 0.6300(8) -0.0179(4) 0.6308(5) 0.032(3) Uiso 1 1 d . . . C20 C 0.6043(8) -0.0550(5) 0.6533(5) 0.040(4) Uiso 1 1 d . . . H20 H 0.5883 -0.0809 0.6370 0.048 Uiso 1 1 calc R . . C21 C 0.6016(7) -0.0552(4) 0.6970(4) 0.030(3) Uiso 1 1 d . . . H21 H 0.5828 -0.0799 0.7124 0.036 Uiso 1 1 calc R . . C22 C 0.6289(7) -0.0158(4) 0.7180(4) 0.031(3) Uiso 1 1 d . . . H22 H 0.6253 -0.0132 0.7486 0.038 Uiso 1 1 calc R . . C23 C 0.6603(7) 0.0190(4) 0.6969(4) 0.021(3) Uiso 1 1 d . . . C24 C 0.7025(7) 0.0606(4) 0.7178(4) 0.028(3) Uiso 1 1 d . . . C25 C 0.6881(7) 0.0707(4) 0.7602(4) 0.024(3) Uiso 1 1 d . . . H25 H 0.6569 0.0525 0.7770 0.028 Uiso 1 1 calc R . . C26 C 0.7256(8) 0.1125(5) 0.7771(5) 0.048(4) Uiso 1 1 d . . . H26 H 0.7206 0.1232 0.8059 0.058 Uiso 1 1 calc R . . C27 C 0.7672(9) 0.1343(5) 0.7487(5) 0.046(4) Uiso 1 1 d . . . H27 H 0.7962 0.1598 0.7591 0.055 Uiso 1 1 calc R . . C28 C 0.7708(7) 0.1217(4) 0.7044(4) 0.029(3) Uiso 1 1 d . . . C29 C 0.8136(8) 0.1448(4) 0.6721(4) 0.030(3) Uiso 1 1 d . . . C30 C 0.8490(9) 0.1893(4) 0.6841(5) 0.051(4) Uiso 1 1 d . . . H30A H 0.8826 0.1987 0.6616 0.077 Uiso 1 1 calc R . . H30B H 0.8812 0.1871 0.7125 0.077 Uiso 1 1 calc R . . H30C H 0.8065 0.2110 0.6862 0.077 Uiso 1 1 calc R . . C31 C 0.8571(7) 0.1462(4) 0.6025(4) 0.027(3) Uiso 1 1 d . . . C32 C 0.8152(8) 0.1786(5) 0.5743(5) 0.040(4) Uiso 1 1 d . . . C33 C 0.8586(8) 0.1961(4) 0.5391(4) 0.036(4) Uiso 1 1 d . . . H33 H 0.8330 0.2174 0.5195 0.044 Uiso 1 1 calc R . . C34 C 0.9336(9) 0.1835(5) 0.5329(5) 0.047(4) Uiso 1 1 d . . . C35 C 0.9694(9) 0.1510(5) 0.5631(5) 0.044(4) Uiso 1 1 d . . . H35 H 1.0223 0.1419 0.5602 0.053 Uiso 1 1 calc R . . C36 C 0.9318(8) 0.1331(4) 0.5947(4) 0.028(3) Uiso 1 1 d . . . C37 C 0.2849(8) 0.0942(4) 0.5951(5) 0.038(4) Uiso 1 1 d . . . H37 H 0.3252 0.0802 0.5777 0.046 Uiso 1 1 calc R . . C38 C 0.2304(9) 0.1209(5) 0.5634(5) 0.060(5) Uiso 1 1 d . . . H38A H 0.1948 0.1386 0.5797 0.089 Uiso 1 1 calc R . . H38B H 0.1992 0.1007 0.5433 0.089 Uiso 1 1 calc R . . H38C H 0.2619 0.1406 0.5465 0.089 Uiso 1 1 calc R . . C39 C 0.2426(8) 0.0549(4) 0.6184(5) 0.045(4) Uiso 1 1 d . . . H39A H 0.2824 0.0375 0.6365 0.068 Uiso 1 1 calc R . . H39B H 0.2148 0.0357 0.5961 0.068 Uiso 1 1 calc R . . H39C H 0.2044 0.0674 0.6371 0.068 Uiso 1 1 calc R . . C40 C 0.5175(8) 0.1967(5) 0.6410(5) 0.043(4) Uiso 1 1 d . . . H40 H 0.5386 0.1842 0.6142 0.052 Uiso 1 1 calc R . . C41 C 0.5047(8) 0.2484(4) 0.6369(5) 0.048(4) Uiso 1 1 d . . . H41A H 0.4643 0.2548 0.6125 0.072 Uiso 1 1 calc R . . H41B H 0.5547 0.2627 0.6315 0.072 Uiso 1 1 calc R . . H41C H 0.4871 0.2599 0.6643 0.072 Uiso 1 1 calc R . . C42 C 0.5755(9) 0.1860(5) 0.6844(5) 0.052(4) Uiso 1 1 d . . . H42A H 0.5498 0.1947 0.7104 0.078 Uiso 1 1 calc R . . H42B H 0.6250 0.2026 0.6836 0.078 Uiso 1 1 calc R . . H42C H 0.5870 0.1540 0.6857 0.078 Uiso 1 1 calc R . . C43 C 0.2873(8) 0.1830(4) 0.7323(4) 0.029(3) Uiso 1 1 d . . . H43 H 0.3207 0.2067 0.7478 0.035 Uiso 1 1 calc R . . C44 C 0.2814(11) 0.1423(6) 0.7675(6) 0.083(6) Uiso 1 1 d . . . H44A H 0.2480 0.1185 0.7538 0.125 Uiso 1 1 calc R . . H44B H 0.2581 0.1534 0.7935 0.125 Uiso 1 1 calc R . . H44C H 0.3346 0.1306 0.7763 0.125 Uiso 1 1 calc R . . C45 C 0.2059(9) 0.2030(5) 0.7207(5) 0.065(5) Uiso 1 1 d . . . H45A H 0.2092 0.2265 0.6988 0.098 Uiso 1 1 calc R . . H45B H 0.1866 0.2156 0.7472 0.098 Uiso 1 1 calc R . . H45C H 0.1692 0.1799 0.7087 0.098 Uiso 1 1 calc R . . C46 C 0.9759(8) 0.1001(4) 0.6295(4) 0.031(3) Uiso 1 1 d . . . H46 H 0.9370 0.0863 0.6479 0.037 Uiso 1 1 calc R . . C47 C 1.0153(8) 0.0630(5) 0.6019(5) 0.056(5) Uiso 1 1 d . . . H47A H 1.0549 0.0766 0.5850 0.084 Uiso 1 1 calc R . . H47B H 0.9743 0.0486 0.5818 0.084 Uiso 1 1 calc R . . H47C H 1.0410 0.0407 0.6220 0.084 Uiso 1 1 calc R . . C48 C 1.0400(9) 0.1228(5) 0.6579(5) 0.063(5) Uiso 1 1 d . . . H48A H 1.0777 0.1363 0.6395 0.095 Uiso 1 1 calc R . . H48B H 1.0677 0.1011 0.6778 0.095 Uiso 1 1 calc R . . H48C H 1.0169 0.1461 0.6751 0.095 Uiso 1 1 calc R . . C49 C 0.9743(10) 0.1980(6) 0.4940(6) 0.067(5) Uiso 1 1 d . . . H49 H 0.9533 0.2288 0.4889 0.080 Uiso 1 1 calc R . . C50 C 0.9573(15) 0.1761(8) 0.4461(8) 0.161(11) Uiso 1 1 d . . . H50A H 0.9922 0.1896 0.4262 0.241 Uiso 1 1 calc R . . H50B H 0.9019 0.1813 0.4349 0.241 Uiso 1 1 calc R . . H50C H 0.9674 0.1441 0.4481 0.241 Uiso 1 1 calc R . . C51 C 1.0606(13) 0.2057(8) 0.5015(8) 0.142(10) Uiso 1 1 d . . . H51A H 1.0706 0.2367 0.5102 0.213 Uiso 1 1 calc R . . H51B H 1.0849 0.1996 0.4744 0.213 Uiso 1 1 calc R . . H51C H 1.0836 0.1859 0.5249 0.213 Uiso 1 1 calc R . . C52 C 0.7324(7) 0.1978(4) 0.5798(4) 0.031(3) Uiso 1 1 d . . . H52 H 0.7109 0.1822 0.6049 0.037 Uiso 1 1 calc R . . C53 C 0.7327(8) 0.2463(4) 0.5887(4) 0.034(4) Uiso 1 1 d . . . H53A H 0.7695 0.2527 0.6147 0.052 Uiso 1 1 calc R . . H53B H 0.6792 0.2559 0.5940 0.052 Uiso 1 1 calc R . . H53C H 0.7495 0.2624 0.5634 0.052 Uiso 1 1 calc R . . C54 C 0.6757(9) 0.1878(5) 0.5366(5) 0.070(5) Uiso 1 1 d . . . H54A H 0.6207 0.1937 0.5419 0.105 Uiso 1 1 calc R . . H54B H 0.6811 0.1566 0.5283 0.105 Uiso 1 1 calc R . . H54C H 0.6902 0.2069 0.5127 0.105 Uiso 1 1 calc R . . C55 C 0.7802(8) 0.0658(5) 0.5331(5) 0.046(4) Uiso 1 1 d . . . C56 C 0.8267(14) 0.0701(8) 0.4893(8) 0.155(10) Uiso 1 1 d . . . H56A H 0.8505 0.0997 0.4883 0.233 Uiso 1 1 calc R . . H56B H 0.7891 0.0656 0.4632 0.233 Uiso 1 1 calc R . . H56C H 0.8684 0.0474 0.4901 0.233 Uiso 1 1 calc R . . Ni1A Ni 0.23901(9) 0.43611(5) 0.65118(5) 0.0210(4) Uani 1 1 d . . . Ni2A Ni 0.00823(9) 0.43442(6) 0.61080(6) 0.0271(5) Uani 1 1 d . . . Cl1A Cl 0.1239(2) 0.39163(9) 0.63093(12) 0.0279(7) Uani 1 1 d . . . Cl2A Cl -0.0955(2) 0.48697(12) 0.59590(11) 0.0333(9) Uani 1 1 d . . . Cl3A Cl 0.34123(19) 0.48850(11) 0.66577(12) 0.0361(9) Uani 1 1 d . . . N1A N -0.0627(5) 0.3757(3) 0.6062(3) 0.018(2) Uiso 1 1 d . . . N2A N 0.0120(6) 0.4146(4) 0.5476(4) 0.033(3) Uiso 1 1 d . . . N3A N 0.0872(6) 0.4861(3) 0.5872(4) 0.029(3) Uiso 1 1 d . . . N4A N 0.1615(5) 0.4838(3) 0.6759(3) 0.015(2) Uiso 1 1 d . . . N5A N 0.2332(6) 0.4172(3) 0.7132(3) 0.022(3) Uiso 1 1 d . . . N6A N 0.3118(6) 0.3750(4) 0.6558(4) 0.038(3) Uiso 1 1 d . . . N7A N 0.2528(7) 0.4445(4) 0.5878(4) 0.041(3) Uiso 1 1 d . . . N8A N -0.0066(5) 0.4413(3) 0.6777(3) 0.015(2) Uiso 1 1 d . . . C1A C -0.0989(7) 0.3513(4) 0.6421(4) 0.023(3) Uiso 1 1 d . . . C2A C -0.0633(7) 0.3225(4) 0.6695(4) 0.021(3) Uiso 1 1 d . . . C3A C -0.1017(8) 0.3070(4) 0.7016(5) 0.038(4) Uiso 1 1 d . . . H3A H -0.0752 0.2856 0.7207 0.046 Uiso 1 1 calc R . . C4A C -0.1793(8) 0.3195(4) 0.7100(5) 0.035(4) Uiso 1 1 d . . . C5A C -0.2117(8) 0.3484(4) 0.6803(4) 0.037(4) Uiso 1 1 d . . . H5A H -0.2640 0.3581 0.6840 0.044 Uiso 1 1 calc R . . C6A C -0.1787(8) 0.3654(4) 0.6457(5) 0.035(4) Uiso 1 1 d . . . C7A C -0.0619(8) 0.3549(4) 0.5695(4) 0.030(4) Uiso 1 1 d . . . C8A C -0.0927(8) 0.3085(4) 0.5570(5) 0.041(4) Uiso 1 1 d . . . H8A1 H -0.1257 0.2976 0.5793 0.062 Uiso 1 1 calc R . . H8A2 H -0.0477 0.2883 0.5552 0.062 Uiso 1 1 calc R . . H8A3 H -0.1243 0.3097 0.5284 0.062 Uiso 1 1 calc R . . C9A C -0.0204(8) 0.3768(4) 0.5347(5) 0.031(4) Uiso 1 1 d . . . C10A C -0.0106(8) 0.3616(5) 0.4927(5) 0.039(4) Uiso 1 1 d . . . H10A H -0.0313 0.3335 0.4833 0.047 Uiso 1 1 calc R . . C11A C 0.0286(8) 0.3870(5) 0.4650(5) 0.045(4) Uiso 1 1 d . . . H11A H 0.0357 0.3766 0.4363 0.054 Uiso 1 1 calc R . . C12A C 0.0591(8) 0.4294(5) 0.4793(5) 0.050(4) Uiso 1 1 d . . . H12A H 0.0832 0.4482 0.4596 0.059 Uiso 1 1 calc R . . C13A C 0.0532(8) 0.4431(4) 0.5230(5) 0.033(4) Uiso 1 1 d . . . C14A C 0.0891(8) 0.4839(5) 0.5436(5) 0.042(4) Uiso 1 1 d . . . C15A C 0.1244(8) 0.5157(4) 0.5183(5) 0.039(4) Uiso 1 1 d . . . H15A H 0.1247 0.5143 0.4873 0.046 Uiso 1 1 calc R . . C16A C 0.1579(7) 0.5486(4) 0.5439(4) 0.028(3) Uiso 1 1 d . . . H16A H 0.1843 0.5716 0.5298 0.033 Uiso 1 1 calc R . . C17A C 0.1570(8) 0.5516(4) 0.5880(4) 0.035(4) Uiso 1 1 d . . . H17A H 0.1814 0.5760 0.6038 0.041 Uiso 1 1 calc R . . C18A C 0.1213(7) 0.5197(4) 0.6089(5) 0.026(3) Uiso 1 1 d . . . C19A C 0.1232(6) 0.5184(4) 0.6561(4) 0.013(3) Uiso 1 1 d . . . C20A C 0.0851(7) 0.5522(4) 0.6789(4) 0.024(3) Uiso 1 1 d . . . H20A H 0.0590 0.5763 0.6636 0.029 Uiso 1 1 calc R . . C21A C 0.0874(8) 0.5488(4) 0.7244(5) 0.035(4) Uiso 1 1 d . . . H21A H 0.0644 0.5710 0.7413 0.042 Uiso 1 1 calc R . . C22A C 0.1225(8) 0.5140(4) 0.7428(5) 0.036(4) Uiso 1 1 d . . . H22A H 0.1229 0.5110 0.7738 0.043 Uiso 1 1 calc R . . C23A C 0.1598(6) 0.4806(3) 0.7202(4) 0.009(3) Uiso 1 1 d . . . C24A C 0.1941(7) 0.4411(4) 0.7397(4) 0.024(3) Uiso 1 1 d . . . C25A C 0.1891(7) 0.4278(4) 0.7826(4) 0.029(3) Uiso 1 1 d . . . H25A H 0.1613 0.4449 0.8022 0.035 Uiso 1 1 calc R . . C26A C 0.2270(7) 0.3878(4) 0.7959(4) 0.024(3) Uiso 1 1 d . . . H26A H 0.2242 0.3781 0.8253 0.029 Uiso 1 1 calc R . . C27A C 0.2683(8) 0.3617(4) 0.7684(4) 0.034(4) Uiso 1 1 d . . . H27A H 0.2941 0.3347 0.7775 0.041 Uiso 1 1 calc R . . C28A C 0.2680(7) 0.3791(4) 0.7266(4) 0.018(3) Uiso 1 1 d . . . C29A C 0.3092(8) 0.3555(5) 0.6940(5) 0.039(4) Uiso 1 1 d . . . C30A C 0.3534(8) 0.3126(4) 0.7044(4) 0.042(4) Uiso 1 1 d . . . H30D H 0.3741 0.3012 0.6778 0.062 Uiso 1 1 calc R . . H30E H 0.3173 0.2906 0.7152 0.062 Uiso 1 1 calc R . . H30F H 0.3975 0.3180 0.7270 0.062 Uiso 1 1 calc R . . C31A C 0.3533(7) 0.3572(4) 0.6200(4) 0.022(3) Uiso 1 1 d . . . C32A C 0.3143(8) 0.3262(4) 0.5898(5) 0.036(4) Uiso 1 1 d . . . C33A C 0.3550(7) 0.3138(4) 0.5538(4) 0.027(3) Uiso 1 1 d . . . H33A H 0.3306 0.2938 0.5325 0.033 Uiso 1 1 calc R . . C34A C 0.4284(7) 0.3299(4) 0.5492(4) 0.024(3) Uiso 1 1 d . . . C35A C 0.4656(8) 0.3597(4) 0.5802(4) 0.036(4) Uiso 1 1 d . . . H35A H 0.5173 0.3701 0.5764 0.043 Uiso 1 1 calc R . . C36A C 0.4283(7) 0.3743(4) 0.6164(4) 0.027(3) Uiso 1 1 d . . . C37A C -0.2236(9) 0.4000(5) 0.6151(5) 0.043(4) Uiso 1 1 d . . . H37A H -0.1833 0.4141 0.5978 0.052 Uiso 1 1 calc R . . C38A C -0.2830(10) 0.3759(5) 0.5819(5) 0.072(6) Uiso 1 1 d . . . H38D H -0.2555 0.3525 0.5671 0.107 Uiso 1 1 calc R . . H38E H -0.3062 0.3972 0.5601 0.107 Uiso 1 1 calc R . . H38F H -0.3251 0.3627 0.5974 0.107 Uiso 1 1 calc R . . C39A C -0.2644(9) 0.4373(5) 0.6367(5) 0.064(5) Uiso 1 1 d . . . H39D H -0.3072 0.4251 0.6524 0.096 Uiso 1 1 calc R . . H39E H -0.2866 0.4582 0.6142 0.096 Uiso 1 1 calc R . . H39F H -0.2260 0.4527 0.6575 0.096 Uiso 1 1 calc R . . C40A C 0.0196(8) 0.3052(4) 0.6632(5) 0.038(4) Uiso 1 1 d . . . H40A H 0.0398 0.3208 0.6377 0.045 Uiso 1 1 calc R . . C41A C 0.0191(8) 0.2558(4) 0.6549(5) 0.042(4) Uiso 1 1 d . . . H41D H -0.0040 0.2405 0.6789 0.063 Uiso 1 1 calc R . . H41E H 0.0735 0.2454 0.6535 0.063 Uiso 1 1 calc R . . H41F H -0.0126 0.2494 0.6271 0.063 Uiso 1 1 calc R . . C42A C 0.0766(8) 0.3144(4) 0.7053(4) 0.037(4) Uiso 1 1 d . . . H42D H 0.0709 0.3454 0.7144 0.055 Uiso 1 1 calc R . . H42E H 0.1314 0.3091 0.6992 0.055 Uiso 1 1 calc R . . H42F H 0.0634 0.2946 0.7290 0.055 Uiso 1 1 calc R . . C43A C -0.2155(9) 0.3029(5) 0.7475(5) 0.046(4) Uiso 1 1 d . . . H43A H -0.1919 0.2729 0.7546 0.056 Uiso 1 1 calc R . . C44A C -0.1995(11) 0.3318(6) 0.7896(6) 0.096(7) Uiso 1 1 d . . . H44D H -0.1426 0.3317 0.7993 0.144 Uiso 1 1 calc R . . H44E H -0.2287 0.3196 0.8129 0.144 Uiso 1 1 calc R . . H44F H -0.2171 0.3623 0.7831 0.144 Uiso 1 1 calc R . . C45A C -0.3029(11) 0.2963(6) 0.7375(6) 0.099(7) Uiso 1 1 d . . . H45D H -0.3284 0.3251 0.7309 0.148 Uiso 1 1 calc R . . H45E H -0.3245 0.2829 0.7629 0.148 Uiso 1 1 calc R . . H45F H -0.3130 0.2766 0.7120 0.148 Uiso 1 1 calc R . . C46A C 0.4732(8) 0.4046(4) 0.6474(4) 0.037(4) Uiso 1 1 d . . . H46A H 0.4345 0.4172 0.6667 0.045 Uiso 1 1 calc R . . C47A C 0.5114(7) 0.4429(4) 0.6277(4) 0.035(4) Uiso 1 1 d . . . H47D H 0.5571 0.4325 0.6132 0.052 Uiso 1 1 calc R . . H47E H 0.5293 0.4643 0.6507 0.052 Uiso 1 1 calc R . . H47F H 0.4732 0.4573 0.6060 0.052 Uiso 1 1 calc R . . C48A C 0.5339(8) 0.3788(5) 0.6770(5) 0.047(4) Uiso 1 1 d . . . H48D H 0.5074 0.3545 0.6912 0.071 Uiso 1 1 calc R . . H48E H 0.5596 0.3986 0.6995 0.071 Uiso 1 1 calc R . . H48F H 0.5739 0.3664 0.6594 0.071 Uiso 1 1 calc R . . C49A C 0.2335(7) 0.3052(4) 0.5936(4) 0.026(3) Uiso 1 1 d . . . H49A H 0.2128 0.3186 0.6201 0.031 Uiso 1 1 calc R . . C50A C 0.2402(8) 0.2553(4) 0.6022(4) 0.034(4) Uiso 1 1 d . . . H50D H 0.2482 0.2399 0.5747 0.051 Uiso 1 1 calc R . . H50E H 0.1914 0.2446 0.6132 0.051 Uiso 1 1 calc R . . H50F H 0.2854 0.2495 0.6240 0.051 Uiso 1 1 calc R . . C51A C 0.1747(8) 0.3176(4) 0.5543(4) 0.037(4) Uiso 1 1 d . . . H51D H 0.1730 0.3500 0.5510 0.055 Uiso 1 1 calc R . . H51E H 0.1218 0.3066 0.5591 0.055 Uiso 1 1 calc R . . H51F H 0.1915 0.3042 0.5275 0.055 Uiso 1 1 calc R . . C52A C 0.4687(8) 0.3171(5) 0.5080(5) 0.044(4) Uiso 1 1 d . . . H52A H 0.4356 0.2938 0.4917 0.053 Uiso 1 1 calc R . . C53A C 0.4724(10) 0.3560(5) 0.4787(5) 0.075(6) Uiso 1 1 d . . . H53D H 0.4198 0.3697 0.4737 0.112 Uiso 1 1 calc R . . H53E H 0.4895 0.3464 0.4505 0.112 Uiso 1 1 calc R . . H53F H 0.5103 0.3777 0.4924 0.112 Uiso 1 1 calc R . . C54A C 0.5540(8) 0.2968(5) 0.5213(5) 0.056(5) Uiso 1 1 d . . . H54D H 0.5759 0.2855 0.4950 0.084 Uiso 1 1 calc R . . H54E H 0.5498 0.2724 0.5422 0.084 Uiso 1 1 calc R . . H54F H 0.5889 0.3199 0.5350 0.084 Uiso 1 1 calc R . . C55A C 0.2704(8) 0.4438(5) 0.5529(5) 0.041(4) Uiso 1 1 d . . . C56A C 0.3037(13) 0.4402(7) 0.5059(7) 0.124(9) Uiso 1 1 d . . . H56D H 0.3548 0.4246 0.5090 0.187 Uiso 1 1 calc R . . H56E H 0.3110 0.4701 0.4942 0.187 Uiso 1 1 calc R . . H56F H 0.2659 0.4237 0.4856 0.187 Uiso 1 1 calc R . . C57A C -0.0318(7) 0.4387(4) 0.7095(4) 0.020(3) Uiso 1 1 d . . . C58A C -0.0588(10) 0.4357(6) 0.7535(5) 0.078(6) Uiso 1 1 d . . . H58A H -0.1167 0.4338 0.7509 0.116 Uiso 1 1 calc R . . H58B H -0.0415 0.4623 0.7704 0.116 Uiso 1 1 calc R . . H58C H -0.0360 0.4092 0.7684 0.116 Uiso 1 1 calc R . . Ni3 Ni 0.37740(14) 0.29877(6) 0.86912(7) 0.0485(5) Uani 1 1 d . . . Cl4 Cl 0.4626(3) 0.33582(12) 0.82873(12) 0.0538(12) Uani 1 1 d . . . Cl5 Cl 0.2962(3) 0.25632(13) 0.82373(13) 0.0673(14) Uani 1 1 d . . . Cl6 Cl 0.4557(3) 0.25612(13) 0.91657(14) 0.0672(14) Uani 1 1 d . . . Cl7 Cl 0.2977(2) 0.33765(12) 0.90975(14) 0.0611(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0172(9) 0.0178(8) 0.0243(10) 0.0011(8) -0.0049(8) -0.0013(8) Ni2 0.0175(9) 0.0197(9) 0.0253(10) -0.0003(8) -0.0056(8) -0.0008(8) Cl1 0.0184(18) 0.0239(18) 0.049(2) -0.0034(16) -0.0131(18) 0.0005(15) Cl2 0.0321(19) 0.0337(19) 0.033(2) 0.0008(16) 0.0122(17) 0.0008(16) Cl3 0.035(2) 0.0242(18) 0.030(2) 0.0012(16) -0.0049(17) -0.0023(16) Ni1A 0.0214(10) 0.0231(10) 0.0168(10) 0.0006(8) -0.0071(8) 0.0012(8) Ni2A 0.0211(10) 0.0302(11) 0.0276(12) -0.0015(9) -0.0097(9) 0.0006(9) Cl1A 0.0213(16) 0.0252(16) 0.0349(19) 0.0007(18) -0.0085(14) -0.0089(17) Cl2A 0.032(2) 0.049(2) 0.019(2) 0.0109(18) 0.0030(17) 0.0079(19) Cl3A 0.029(2) 0.032(2) 0.047(3) 0.0005(18) -0.0009(19) -0.0083(16) Ni3 0.0732(14) 0.0337(10) 0.0338(11) -0.0020(11) -0.0185(10) 0.0063(13) Cl4 0.081(3) 0.038(2) 0.040(3) 0.0047(19) -0.009(2) 0.005(2) Cl5 0.103(4) 0.047(3) 0.043(3) -0.006(2) -0.035(3) -0.003(3) Cl6 0.107(4) 0.036(2) 0.052(3) -0.001(2) -0.024(3) 0.004(2) Cl7 0.062(3) 0.038(2) 0.077(3) -0.011(2) -0.027(3) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.937(11) . ? Ni1 N3 2.128(10) . ? Ni1 N1 2.172(9) . ? Ni1 Cl2 2.213(4) . ? Ni1 Cl1 2.276(4) . ? Ni2 N5 1.880(9) . ? Ni2 N7 2.024(11) . ? Ni2 N4 2.156(10) . ? Ni2 N6 2.218(10) . ? Ni2 Cl3 2.333(4) . ? Ni2 Cl1 2.422(4) . ? N1 C7 1.257(13) . ? N1 C1 1.390(14) . ? N2 C13 1.392(15) . ? N2 C9 1.413(15) . ? N3 C14 1.367(15) . ? N3 C18 1.407(15) . ? N4 C19 1.347(14) . ? N4 C23 1.391(14) . ? N5 C24 1.289(13) . ? N5 C28 1.411(14) . ? N6 C29 1.271(14) . ? N6 C31 1.360(14) . ? N7 C55 1.070(15) . ? C1 C6 1.403(16) . ? C1 C2 1.409(17) . ? C2 C3 1.423(16) . ? C2 C40 1.553(17) . ? C3 C4 1.410(17) . ? C3 H3 0.9500 . ? C4 C5 1.409(17) . ? C4 C43 1.423(16) . ? C5 C6 1.392(15) . ? C5 H5 0.9500 . ? C6 C37 1.509(16) . ? C7 C9 1.446(14) . ? C7 C8 1.501(14) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.378(16) . ? C10 C11 1.362(16) . ? C10 H10 0.9500 . ? C11 C12 1.436(16) . ? C11 H11 0.9500 . ? C12 C13 1.389(16) . ? C12 H12 0.9500 . ? C13 C14 1.457(17) . ? C14 C15 1.421(16) . ? C15 C16 1.416(16) . ? C15 H15 0.9500 . ? C16 C17 1.310(15) . ? C16 H16 0.9500 . ? C17 C18 1.337(16) . ? C17 H17 0.9500 . ? C18 C19 1.469(17) . ? C19 C20 1.406(16) . ? C20 C21 1.341(16) . ? C20 H20 0.9500 . ? C21 C22 1.405(16) . ? C21 H21 0.9500 . ? C22 C23 1.364(15) . ? C22 H22 0.9500 . ? C23 C24 1.550(16) . ? C24 C25 1.376(15) . ? C25 C26 1.478(17) . ? C25 H25 0.9500 . ? C26 C27 1.343(17) . ? C26 H26 0.9500 . ? C27 C28 1.416(17) . ? C27 H27 0.9500 . ? C28 C29 1.459(16) . ? C29 C30 1.497(17) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.370(16) . ? C31 C32 1.441(17) . ? C32 C33 1.462(17) . ? C32 C52 1.543(17) . ? C33 C34 1.359(18) . ? C33 H33 0.9500 . ? C34 C35 1.436(18) . ? C34 C49 1.500(19) . ? C35 C36 1.325(16) . ? C35 H35 0.9500 . ? C36 C46 1.587(16) . ? C37 C38 1.502(18) . ? C37 C39 1.588(16) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.574(17) . ? C40 C42 1.602(18) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C45 1.514(18) . ? C43 C44 1.642(18) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C48 1.489(18) . ? C46 C47 1.586(16) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C51 1.48(2) . ? C49 C50 1.60(2) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.485(15) . ? C52 C54 1.583(18) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.62(2) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? Ni1A N7A 1.992(12) . ? Ni1A N5A 1.992(10) . ? Ni1A N4A 2.135(9) . ? Ni1A N6A 2.210(11) . ? Ni1A Cl3A 2.352(4) . ? Ni1A Cl1A 2.395(4) . ? Ni2A N2A 2.030(11) . ? Ni2A N8A 2.098(9) . ? Ni2A N1A 2.133(9) . ? Ni2A N3A 2.218(10) . ? Ni2A Cl2A 2.375(4) . ? Ni2A Cl1A 2.375(4) . ? N1A C7A 1.287(14) . ? N1A C1A 1.501(14) . ? N2A C9A 1.307(15) . ? N2A C13A 1.379(15) . ? N3A C18A 1.310(15) . ? N3A C14A 1.340(15) . ? N4A C19A 1.339(13) . ? N4A C23A 1.362(12) . ? N5A C24A 1.312(13) . ? N5A C28A 1.336(14) . ? N6A C29A 1.311(16) . ? N6A C31A 1.462(14) . ? N7A C55A 1.139(16) . ? N8A C57A 1.102(13) . ? C1A C2A 1.311(15) . ? C1A C6A 1.434(16) . ? C2A C3A 1.319(15) . ? C2A C40A 1.529(16) . ? C3A C4A 1.417(17) . ? C3A H3A 0.9500 . ? C4A C5A 1.337(17) . ? C4A C43A 1.443(17) . ? C5A C6A 1.346(16) . ? C5A H5A 0.9500 . ? C6A C37A 1.546(18) . ? C7A C9A 1.490(16) . ? C7A C8A 1.526(16) . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A C10A 1.388(17) . ? C10A C11A 1.364(17) . ? C10A H10A 0.9500 . ? C11A C12A 1.428(18) . ? C11A H11A 0.9500 . ? C12A C13A 1.411(17) . ? C12A H12A 0.9500 . ? C13A C14A 1.481(18) . ? C14A C15A 1.402(17) . ? C15A C16A 1.352(16) . ? C15A H15A 0.9500 . ? C16A C17A 1.353(16) . ? C16A H16A 0.9500 . ? C17A C18A 1.331(16) . ? C17A H17A 0.9500 . ? C18A C19A 1.442(14) . ? C19A C20A 1.426(14) . ? C20A C21A 1.390(16) . ? C20A H20A 0.9500 . ? C21A C22A 1.306(16) . ? C21A H21A 0.9500 . ? C22A C23A 1.406(15) . ? C22A H22A 0.9500 . ? C23A C24A 1.428(15) . ? C24A C25A 1.381(15) . ? C25A C26A 1.404(15) . ? C25A H25A 0.9500 . ? C26A C27A 1.391(15) . ? C26A H26A 0.9500 . ? C27A C28A 1.381(16) . ? C27A H27A 0.9500 . ? C28A C29A 1.460(16) . ? C29A C30A 1.512(17) . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C31A C36A 1.388(16) . ? C31A C32A 1.427(17) . ? C32A C33A 1.408(16) . ? C32A C49A 1.524(17) . ? C33A C34A 1.357(15) . ? C33A H33A 0.9500 . ? C34A C35A 1.407(16) . ? C34A C52A 1.540(16) . ? C35A C36A 1.401(16) . ? C35A H35A 0.9500 . ? C36A C46A 1.471(17) . ? C37A C39A 1.505(17) . ? C37A C38A 1.538(19) . ? C37A H37A 1.0000 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 0.9800 . ? C40A C41A 1.507(17) . ? C40A C42A 1.557(17) . ? C40A H40A 1.0000 . ? C41A H41D 0.9800 . ? C41A H41E 0.9800 . ? C41A H41F 0.9800 . ? C42A H42D 0.9800 . ? C42A H42E 0.9800 . ? C42A H42F 0.9800 . ? C43A C45A 1.50(2) . ? C43A C44A 1.55(2) . ? C43A H43A 1.0000 . ? C44A H44D 0.9800 . ? C44A H44E 0.9800 . ? C44A H44F 0.9800 . ? C45A H45D 0.9800 . ? C45A H45E 0.9800 . ? C45A H45F 0.9800 . ? C46A C47A 1.480(15) . ? C46A C48A 1.516(17) . ? C46A H46A 1.0000 . ? C47A H47D 0.9800 . ? C47A H47E 0.9800 . ? C47A H47F 0.9800 . ? C48A H48D 0.9800 . ? C48A H48E 0.9800 . ? C48A H48F 0.9800 . ? C49A C50A 1.526(15) . ? C49A C51A 1.530(16) . ? C49A H49A 1.0000 . ? C50A H50D 0.9800 . ? C50A H50E 0.9800 . ? C50A H50F 0.9800 . ? C51A H51D 0.9800 . ? C51A H51E 0.9800 . ? C51A H51F 0.9800 . ? C52A C53A 1.479(18) . ? C52A C54A 1.585(18) . ? C52A H52A 1.0000 . ? C53A H53D 0.9800 . ? C53A H53E 0.9800 . ? C53A H53F 0.9800 . ? C54A H54D 0.9800 . ? C54A H54E 0.9800 . ? C54A H54F 0.9800 . ? C55A C56A 1.60(2) . ? C56A H56D 0.9800 . ? C56A H56E 0.9800 . ? C56A H56F 0.9800 . ? C57A C58A 1.467(17) . ? C58A H58A 0.9800 . ? C58A H58B 0.9800 . ? C58A H58C 0.9800 . ? Ni3 Cl5 2.251(5) . ? Ni3 Cl7 2.254(5) . ? Ni3 Cl6 2.265(5) . ? Ni3 Cl4 2.284(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N3 79.6(4) . . ? N2 Ni1 N1 77.5(4) . . ? N3 Ni1 N1 157.0(4) . . ? N2 Ni1 Cl2 132.4(3) . . ? N3 Ni1 Cl2 96.1(3) . . ? N1 Ni1 Cl2 99.5(3) . . ? N2 Ni1 Cl1 96.8(3) . . ? N3 Ni1 Cl1 92.8(3) . . ? N1 Ni1 Cl1 89.7(3) . . ? Cl2 Ni1 Cl1 130.78(15) . . ? N5 Ni2 N7 170.1(4) . . ? N5 Ni2 N4 75.5(4) . . ? N7 Ni2 N4 113.7(4) . . ? N5 Ni2 N6 79.9(4) . . ? N7 Ni2 N6 90.7(4) . . ? N4 Ni2 N6 154.8(4) . . ? N5 Ni2 Cl3 96.6(3) . . ? N7 Ni2 Cl3 87.9(3) . . ? N4 Ni2 Cl3 86.7(3) . . ? N6 Ni2 Cl3 100.9(3) . . ? N5 Ni2 Cl1 86.3(3) . . ? N7 Ni2 Cl1 90.6(3) . . ? N4 Ni2 Cl1 85.6(3) . . ? N6 Ni2 Cl1 88.2(3) . . ? Cl3 Ni2 Cl1 170.78(13) . . ? Ni1 Cl1 Ni2 111.29(14) . . ? C7 N1 C1 120.7(10) . . ? C7 N1 Ni1 112.7(8) . . ? C1 N1 Ni1 126.6(8) . . ? C13 N2 C9 119.4(11) . . ? C13 N2 Ni1 121.4(9) . . ? C9 N2 Ni1 118.6(9) . . ? C14 N3 C18 119.7(11) . . ? C14 N3 Ni1 109.5(8) . . ? C18 N3 Ni1 130.3(9) . . ? C19 N4 C23 115.6(11) . . ? C19 N4 Ni2 130.1(9) . . ? C23 N4 Ni2 113.5(8) . . ? C24 N5 C28 111.4(10) . . ? C24 N5 Ni2 129.9(8) . . ? C28 N5 Ni2 118.7(8) . . ? C29 N6 C31 123.8(11) . . ? C29 N6 Ni2 108.9(9) . . ? C31 N6 Ni2 126.7(8) . . ? C55 N7 Ni2 161.5(12) . . ? N1 C1 C6 120.8(12) . . ? N1 C1 C2 121.9(12) . . ? C6 C1 C2 117.2(12) . . ? C1 C2 C3 121.5(12) . . ? C1 C2 C40 119.4(12) . . ? C3 C2 C40 119.0(12) . . ? C4 C3 C2 121.2(13) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 115.1(13) . . ? C5 C4 C43 122.5(13) . . ? C3 C4 C43 122.0(13) . . ? C6 C5 C4 124.2(13) . . ? C6 C5 H5 117.9 . . ? C4 C5 H5 117.9 . . ? C5 C6 C1 120.2(12) . . ? C5 C6 C37 118.7(11) . . ? C1 C6 C37 121.1(12) . . ? N1 C7 C9 119.0(10) . . ? N1 C7 C8 126.7(10) . . ? C9 C7 C8 114.2(10) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N2 116.2(11) . . ? C10 C9 C7 132.3(12) . . ? N2 C9 C7 111.2(11) . . ? C11 C10 C9 125.1(13) . . ? C11 C10 H10 117.5 . . ? C9 C10 H10 117.5 . . ? C10 C11 C12 119.6(13) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 115.5(12) . . ? C13 C12 H12 122.3 . . ? C11 C12 H12 122.3 . . ? C12 C13 N2 124.1(12) . . ? C12 C13 C14 126.6(13) . . ? N2 C13 C14 109.0(12) . . ? N3 C14 C15 120.2(12) . . ? N3 C14 C13 120.3(12) . . ? C15 C14 C13 119.4(13) . . ? C16 C15 C14 117.3(13) . . ? C16 C15 H15 121.3 . . ? C14 C15 H15 121.3 . . ? C17 C16 C15 119.4(13) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 125.2(14) . . ? C16 C17 H17 117.4 . . ? C18 C17 H17 117.4 . . ? C17 C18 N3 118.1(13) . . ? C17 C18 C19 128.6(13) . . ? N3 C18 C19 113.0(12) . . ? N4 C19 C20 122.5(14) . . ? N4 C19 C18 116.5(12) . . ? C20 C19 C18 120.4(13) . . ? C21 C20 C19 122.4(14) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C20 C21 C22 114.1(13) . . ? C20 C21 H21 122.9 . . ? C22 C21 H21 122.9 . . ? C23 C22 C21 123.9(13) . . ? C23 C22 H22 118.1 . . ? C21 C22 H22 118.1 . . ? C22 C23 N4 120.5(11) . . ? C22 C23 C24 127.6(12) . . ? N4 C23 C24 111.5(10) . . ? N5 C24 C25 133.7(12) . . ? N5 C24 C23 108.8(11) . . ? C25 C24 C23 116.7(11) . . ? C24 C25 C26 114.0(12) . . ? C24 C25 H25 123.0 . . ? C26 C25 H25 123.0 . . ? C27 C26 C25 115.0(14) . . ? C27 C26 H26 122.5 . . ? C25 C26 H26 122.5 . . ? C26 C27 C28 124.5(15) . . ? C26 C27 H27 117.7 . . ? C28 C27 H27 117.7 . . ? N5 C28 C27 120.7(12) . . ? N5 C28 C29 112.6(11) . . ? C27 C28 C29 126.5(13) . . ? N6 C29 C28 119.9(12) . . ? N6 C29 C30 121.5(12) . . ? C28 C29 C30 118.2(12) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N6 C31 C36 126.6(12) . . ? N6 C31 C32 113.4(11) . . ? C36 C31 C32 119.9(12) . . ? C31 C32 C33 115.5(12) . . ? C31 C32 C52 126.0(12) . . ? C33 C32 C52 118.4(12) . . ? C34 C33 C32 123.2(14) . . ? C34 C33 H33 118.4 . . ? C32 C33 H33 118.4 . . ? C33 C34 C35 116.3(14) . . ? C33 C34 C49 122.6(15) . . ? C35 C34 C49 120.7(14) . . ? C36 C35 C34 122.8(14) . . ? C36 C35 H35 118.6 . . ? C34 C35 H35 118.6 . . ? C35 C36 C31 122.2(13) . . ? C35 C36 C46 120.9(12) . . ? C31 C36 C46 116.4(11) . . ? C38 C37 C6 108.3(11) . . ? C38 C37 C39 114.2(12) . . ? C6 C37 C39 113.3(11) . . ? C38 C37 H37 106.9 . . ? C6 C37 H37 106.9 . . ? C39 C37 H37 106.9 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C2 C40 C41 109.5(11) . . ? C2 C40 C42 103.6(11) . . ? C41 C40 C42 109.4(11) . . ? C2 C40 H40 111.3 . . ? C41 C40 H40 111.3 . . ? C42 C40 H40 111.3 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C4 C43 C45 113.0(12) . . ? C4 C43 C44 113.5(11) . . ? C45 C43 C44 109.6(11) . . ? C4 C43 H43 106.7 . . ? C45 C43 H43 106.7 . . ? C44 C43 H43 106.7 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C48 C46 C47 108.2(11) . . ? C48 C46 C36 111.8(11) . . ? C47 C46 C36 106.3(11) . . ? C48 C46 H46 110.2 . . ? C47 C46 H46 110.2 . . ? C36 C46 H46 110.2 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C51 C49 C34 116.7(17) . . ? C51 C49 C50 106.8(16) . . ? C34 C49 C50 123.4(16) . . ? C51 C49 H49 102.1 . . ? C34 C49 H49 102.1 . . ? C50 C49 H49 102.1 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C32 113.7(11) . . ? C53 C52 C54 109.4(11) . . ? C32 C52 C54 108.8(11) . . ? C53 C52 H52 108.3 . . ? C32 C52 H52 108.3 . . ? C54 C52 H52 108.3 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N7 C55 C56 172.3(17) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N7A Ni1A N5A 170.0(4) . . ? N7A Ni1A N4A 113.3(4) . . ? N5A Ni1A N4A 76.3(4) . . ? N7A Ni1A N6A 92.8(4) . . ? N5A Ni1A N6A 77.5(4) . . ? N4A Ni1A N6A 153.6(4) . . ? N7A Ni1A Cl3A 86.7(3) . . ? N5A Ni1A Cl3A 96.7(3) . . ? N4A Ni1A Cl3A 87.2(3) . . ? N6A Ni1A Cl3A 98.6(3) . . ? N7A Ni1A Cl1A 89.5(3) . . ? N5A Ni1A Cl1A 88.3(3) . . ? N4A Ni1A Cl1A 87.3(3) . . ? N6A Ni1A Cl1A 89.3(3) . . ? Cl3A Ni1A Cl1A 171.47(14) . . ? N2A Ni2A N8A 167.5(4) . . ? N2A Ni2A N1A 76.4(4) . . ? N8A Ni2A N1A 91.3(4) . . ? N2A Ni2A N3A 79.6(4) . . ? N8A Ni2A N3A 112.6(4) . . ? N1A Ni2A N3A 156.0(4) . . ? N2A Ni2A Cl2A 96.1(3) . . ? N8A Ni2A Cl2A 87.9(3) . . ? N1A Ni2A Cl2A 97.8(3) . . ? N3A Ni2A Cl2A 86.0(3) . . ? N2A Ni2A Cl1A 89.0(3) . . ? N8A Ni2A Cl1A 88.7(3) . . ? N1A Ni2A Cl1A 90.8(3) . . ? N3A Ni2A Cl1A 87.4(3) . . ? Cl2A Ni2A Cl1A 170.77(14) . . ? Ni2A Cl1A Ni1A 113.21(13) . . ? C7A N1A C1A 116.1(10) . . ? C7A N1A Ni2A 114.0(8) . . ? C1A N1A Ni2A 128.7(8) . . ? C9A N2A C13A 126.7(12) . . ? C9A N2A Ni2A 119.4(10) . . ? C13A N2A Ni2A 113.8(9) . . ? C18A N3A C14A 119.1(12) . . ? C18A N3A Ni2A 128.8(10) . . ? C14A N3A Ni2A 111.4(9) . . ? C19A N4A C23A 116.7(10) . . ? C19A N4A Ni1A 130.5(8) . . ? C23A N4A Ni1A 112.3(7) . . ? C24A N5A C28A 120.9(11) . . ? C24A N5A Ni1A 120.7(9) . . ? C28A N5A Ni1A 118.4(8) . . ? C29A N6A C31A 124.3(12) . . ? C29A N6A Ni1A 111.2(10) . . ? C31A N6A Ni1A 124.4(8) . . ? C55A N7A Ni1A 168.1(12) . . ? C57A N8A Ni2A 161.4(9) . . ? C2A C1A C6A 121.5(12) . . ? C2A C1A N1A 126.6(11) . . ? C6A C1A N1A 111.7(11) . . ? C1A C2A C3A 118.8(12) . . ? C1A C2A C40A 121.0(12) . . ? C3A C2A C40A 120.1(12) . . ? C2A C3A C4A 125.4(14) . . ? C2A C3A H3A 117.3 . . ? C4A C3A H3A 117.3 . . ? C5A C4A C3A 112.0(13) . . ? C5A C4A C43A 126.1(14) . . ? C3A C4A C43A 121.9(13) . . ? C4A C5A C6A 127.4(14) . . ? C4A C5A H5A 116.3 . . ? C6A C5A H5A 116.3 . . ? C5A C6A C1A 114.8(13) . . ? C5A C6A C37A 120.9(13) . . ? C1A C6A C37A 124.2(12) . . ? N1A C7A C9A 117.1(12) . . ? N1A C7A C8A 129.2(12) . . ? C9A C7A C8A 113.5(12) . . ? C7A C8A H8A1 109.5 . . ? C7A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C7A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? N2A C9A C10A 118.8(13) . . ? N2A C9A C7A 112.5(12) . . ? C10A C9A C7A 128.7(13) . . ? C11A C10A C9A 120.1(14) . . ? C11A C10A H10A 119.9 . . ? C9A C10A H10A 119.9 . . ? C10A C11A C12A 119.6(15) . . ? C10A C11A H11A 120.2 . . ? C12A C11A H11A 120.2 . . ? C13A C12A C11A 119.7(14) . . ? C13A C12A H12A 120.2 . . ? C11A C12A H12A 120.2 . . ? N2A C13A C12A 115.0(13) . . ? N2A C13A C14A 119.4(13) . . ? C12A C13A C14A 125.5(14) . . ? N3A C14A C15A 124.8(14) . . ? N3A C14A C13A 114.5(13) . . ? C15A C14A C13A 120.7(14) . . ? C16A C15A C14A 111.0(14) . . ? C16A C15A H15A 124.5 . . ? C14A C15A H15A 124.5 . . ? C15A C16A C17A 125.4(13) . . ? C15A C16A H16A 117.3 . . ? C17A C16A H16A 117.3 . . ? C18A C17A C16A 118.8(14) . . ? C18A C17A H17A 120.6 . . ? C16A C17A H17A 120.6 . . ? N3A C18A C17A 120.9(14) . . ? N3A C18A C19A 116.6(12) . . ? C17A C18A C19A 122.3(13) . . ? N4A C19A C20A 123.7(11) . . ? N4A C19A C18A 115.9(11) . . ? C20A C19A C18A 120.4(11) . . ? C21A C20A C19A 118.1(12) . . ? C21A C20A H20A 120.9 . . ? C19A C20A H20A 120.9 . . ? C22A C21A C20A 117.1(14) . . ? C22A C21A H21A 121.5 . . ? C20A C21A H21A 121.5 . . ? C21A C22A C23A 124.7(14) . . ? C21A C22A H22A 117.7 . . ? C23A C22A H22A 117.7 . . ? N4A C23A C22A 119.6(11) . . ? N4A C23A C24A 115.3(10) . . ? C22A C23A C24A 125.0(11) . . ? N5A C24A C25A 120.8(12) . . ? N5A C24A C23A 113.9(11) . . ? C25A C24A C23A 125.3(12) . . ? C24A C25A C26A 117.0(12) . . ? C24A C25A H25A 121.5 . . ? C26A C25A H25A 121.5 . . ? C27A C26A C25A 123.4(13) . . ? C27A C26A H26A 118.3 . . ? C25A C26A H26A 118.3 . . ? C28A C27A C26A 113.0(13) . . ? C28A C27A H27A 123.5 . . ? C26A C27A H27A 123.5 . . ? N5A C28A C27A 124.8(12) . . ? N5A C28A C29A 115.7(12) . . ? C27A C28A C29A 119.5(12) . . ? N6A C29A C28A 116.9(13) . . ? N6A C29A C30A 120.7(13) . . ? C28A C29A C30A 122.1(13) . . ? C29A C30A H30D 109.5 . . ? C29A C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? C29A C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? C36A C31A C32A 124.0(12) . . ? C36A C31A N6A 115.9(11) . . ? C32A C31A N6A 119.9(11) . . ? C33A C32A C31A 116.7(12) . . ? C33A C32A C49A 117.6(12) . . ? C31A C32A C49A 125.7(12) . . ? C34A C33A C32A 120.9(13) . . ? C34A C33A H33A 119.6 . . ? C32A C33A H33A 119.6 . . ? C33A C34A C35A 120.7(12) . . ? C33A C34A C52A 118.9(12) . . ? C35A C34A C52A 120.3(12) . . ? C36A C35A C34A 121.9(13) . . ? C36A C35A H35A 119.1 . . ? C34A C35A H35A 119.1 . . ? C31A C36A C35A 115.8(12) . . ? C31A C36A C46A 126.7(12) . . ? C35A C36A C46A 117.4(12) . . ? C39A C37A C38A 110.0(13) . . ? C39A C37A C6A 117.1(12) . . ? C38A C37A C6A 109.5(12) . . ? C39A C37A H37A 106.6 . . ? C38A C37A H37A 106.6 . . ? C6A C37A H37A 106.6 . . ? C37A C38A H38D 109.5 . . ? C37A C38A H38E 109.5 . . ? H38D C38A H38E 109.5 . . ? C37A C38A H38F 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? C37A C39A H39D 109.5 . . ? C37A C39A H39E 109.5 . . ? H39D C39A H39E 109.5 . . ? C37A C39A H39F 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C41A C40A C2A 111.6(11) . . ? C41A C40A C42A 107.9(11) . . ? C2A C40A C42A 109.7(11) . . ? C41A C40A H40A 109.2 . . ? C2A C40A H40A 109.2 . . ? C42A C40A H40A 109.2 . . ? C40A C41A H41D 109.5 . . ? C40A C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? C40A C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? C40A C42A H42D 109.5 . . ? C40A C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C40A C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? C4A C43A C45A 112.0(14) . . ? C4A C43A C44A 114.2(13) . . ? C45A C43A C44A 109.3(14) . . ? C4A C43A H43A 107.0 . . ? C45A C43A H43A 107.0 . . ? C44A C43A H43A 107.0 . . ? C43A C44A H44D 109.5 . . ? C43A C44A H44E 109.5 . . ? H44D C44A H44E 109.5 . . ? C43A C44A H44F 109.5 . . ? H44D C44A H44F 109.5 . . ? H44E C44A H44F 109.5 . . ? C43A C45A H45D 109.5 . . ? C43A C45A H45E 109.5 . . ? H45D C45A H45E 109.5 . . ? C43A C45A H45F 109.5 . . ? H45D C45A H45F 109.5 . . ? H45E C45A H45F 109.5 . . ? C36A C46A C47A 116.0(12) . . ? C36A C46A C48A 110.0(11) . . ? C47A C46A C48A 110.2(11) . . ? C36A C46A H46A 106.7 . . ? C47A C46A H46A 106.7 . . ? C48A C46A H46A 106.7 . . ? C46A C47A H47D 109.5 . . ? C46A C47A H47E 109.5 . . ? H47D C47A H47E 109.5 . . ? C46A C47A H47F 109.5 . . ? H47D C47A H47F 109.5 . . ? H47E C47A H47F 109.5 . . ? C46A C48A H48D 109.5 . . ? C46A C48A H48E 109.5 . . ? H48D C48A H48E 109.5 . . ? C46A C48A H48F 109.5 . . ? H48D C48A H48F 109.5 . . ? H48E C48A H48F 109.5 . . ? C32A C49A C50A 111.7(11) . . ? C32A C49A C51A 111.1(10) . . ? C50A C49A C51A 114.0(11) . . ? C32A C49A H49A 106.5 . . ? C50A C49A H49A 106.5 . . ? C51A C49A H49A 106.5 . . ? C49A C50A H50D 109.5 . . ? C49A C50A H50E 109.5 . . ? H50D C50A H50E 109.5 . . ? C49A C50A H50F 109.5 . . ? H50D C50A H50F 109.5 . . ? H50E C50A H50F 109.5 . . ? C49A C51A H51D 109.5 . . ? C49A C51A H51E 109.5 . . ? H51D C51A H51E 109.5 . . ? C49A C51A H51F 109.5 . . ? H51D C51A H51F 109.5 . . ? H51E C51A H51F 109.5 . . ? C53A C52A C34A 110.4(12) . . ? C53A C52A C54A 111.6(13) . . ? C34A C52A C54A 110.7(12) . . ? C53A C52A H52A 108.0 . . ? C34A C52A H52A 108.0 . . ? C54A C52A H52A 108.0 . . ? C52A C53A H53D 109.5 . . ? C52A C53A H53E 109.5 . . ? H53D C53A H53E 109.5 . . ? C52A C53A H53F 109.5 . . ? H53D C53A H53F 109.5 . . ? H53E C53A H53F 109.5 . . ? C52A C54A H54D 109.5 . . ? C52A C54A H54E 109.5 . . ? H54D C54A H54E 109.5 . . ? C52A C54A H54F 109.5 . . ? H54D C54A H54F 109.5 . . ? H54E C54A H54F 109.5 . . ? N7A C55A C56A 173.8(16) . . ? C55A C56A H56D 109.5 . . ? C55A C56A H56E 109.5 . . ? H56D C56A H56E 109.5 . . ? C55A C56A H56F 109.5 . . ? H56D C56A H56F 109.5 . . ? H56E C56A H56F 109.5 . . ? N8A C57A C58A 175.3(14) . . ? C57A C58A H58A 109.5 . . ? C57A C58A H58B 109.5 . . ? H58A C58A H58B 109.5 . . ? C57A C58A H58C 109.5 . . ? H58A C58A H58C 109.5 . . ? H58B C58A H58C 109.5 . . ? Cl5 Ni3 Cl7 105.76(19) . . ? Cl5 Ni3 Cl6 110.89(15) . . ? Cl7 Ni3 Cl6 106.61(18) . . ? Cl5 Ni3 Cl4 108.90(18) . . ? Cl7 Ni3 Cl4 119.48(15) . . ? Cl6 Ni3 Cl4 105.15(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 Cl1 Ni2 -106.6(3) . . . . ? N3 Ni1 Cl1 Ni2 -26.8(3) . . . . ? N1 Ni1 Cl1 Ni2 176.0(3) . . . . ? Cl2 Ni1 Cl1 Ni2 73.7(2) . . . . ? N5 Ni2 Cl1 Ni1 -112.7(3) . . . . ? N7 Ni2 Cl1 Ni1 76.7(3) . . . . ? N4 Ni2 Cl1 Ni1 -37.0(3) . . . . ? N6 Ni2 Cl1 Ni1 167.3(3) . . . . ? Cl3 Ni2 Cl1 Ni1 -4.0(10) . . . . ? N2 Ni1 N1 C7 -6.9(8) . . . . ? N3 Ni1 N1 C7 -6.4(15) . . . . ? Cl2 Ni1 N1 C7 -138.4(8) . . . . ? Cl1 Ni1 N1 C7 90.2(8) . . . . ? N2 Ni1 N1 C1 174.9(10) . . . . ? N3 Ni1 N1 C1 175.4(10) . . . . ? Cl2 Ni1 N1 C1 43.4(10) . . . . ? Cl1 Ni1 N1 C1 -88.0(10) . . . . ? N3 Ni1 N2 C13 1.4(9) . . . . ? N1 Ni1 N2 C13 -178.8(10) . . . . ? Cl2 Ni1 N2 C13 -87.3(10) . . . . ? Cl1 Ni1 N2 C13 93.0(9) . . . . ? N3 Ni1 N2 C9 -170.2(10) . . . . ? N1 Ni1 N2 C9 9.6(9) . . . . ? Cl2 Ni1 N2 C9 101.1(9) . . . . ? Cl1 Ni1 N2 C9 -78.6(9) . . . . ? N2 Ni1 N3 C14 -3.4(8) . . . . ? N1 Ni1 N3 C14 -4.0(15) . . . . ? Cl2 Ni1 N3 C14 128.6(8) . . . . ? Cl1 Ni1 N3 C14 -99.9(8) . . . . ? N2 Ni1 N3 C18 -175.1(12) . . . . ? N1 Ni1 N3 C18 -175.6(10) . . . . ? Cl2 Ni1 N3 C18 -43.0(11) . . . . ? Cl1 Ni1 N3 C18 88.5(11) . . . . ? N5 Ni2 N4 C19 -177.6(11) . . . . ? N7 Ni2 N4 C19 6.4(12) . . . . ? N6 Ni2 N4 C19 171.2(10) . . . . ? Cl3 Ni2 N4 C19 -79.9(11) . . . . ? Cl1 Ni2 N4 C19 95.1(11) . . . . ? N5 Ni2 N4 C23 -8.2(8) . . . . ? N7 Ni2 N4 C23 175.8(8) . . . . ? N6 Ni2 N4 C23 -19.5(13) . . . . ? Cl3 Ni2 N4 C23 89.5(8) . . . . ? Cl1 Ni2 N4 C23 -95.5(8) . . . . ? N7 Ni2 N5 C24 165(2) . . . . ? N4 Ni2 N5 C24 6.9(10) . . . . ? N6 Ni2 N5 C24 -178.0(11) . . . . ? Cl3 Ni2 N5 C24 -78.0(10) . . . . ? Cl1 Ni2 N5 C24 93.2(10) . . . . ? N7 Ni2 N5 C28 -14(3) . . . . ? N4 Ni2 N5 C28 -172.5(9) . . . . ? N6 Ni2 N5 C28 2.7(8) . . . . ? Cl3 Ni2 N5 C28 102.7(8) . . . . ? Cl1 Ni2 N5 C28 -86.1(8) . . . . ? N5 Ni2 N6 C29 -0.7(9) . . . . ? N7 Ni2 N6 C29 176.4(9) . . . . ? N4 Ni2 N6 C29 10.3(14) . . . . ? Cl3 Ni2 N6 C29 -95.6(9) . . . . ? Cl1 Ni2 N6 C29 85.8(9) . . . . ? N5 Ni2 N6 C31 171.1(10) . . . . ? N7 Ni2 N6 C31 -11.7(10) . . . . ? N4 Ni2 N6 C31 -177.8(9) . . . . ? Cl3 Ni2 N6 C31 76.3(10) . . . . ? Cl1 Ni2 N6 C31 -102.3(10) . . . . ? N5 Ni2 N7 C55 39(5) . . . . ? N4 Ni2 N7 C55 -164(4) . . . . ? N6 Ni2 N7 C55 22(4) . . . . ? Cl3 Ni2 N7 C55 -79(4) . . . . ? Cl1 Ni2 N7 C55 111(4) . . . . ? C7 N1 C1 C6 96.4(15) . . . . ? Ni1 N1 C1 C6 -85.6(14) . . . . ? C7 N1 C1 C2 -87.9(16) . . . . ? Ni1 N1 C1 C2 90.1(14) . . . . ? N1 C1 C2 C3 -172.4(11) . . . . ? C6 C1 C2 C3 3(2) . . . . ? N1 C1 C2 C40 9.5(19) . . . . ? C6 C1 C2 C40 -174.6(11) . . . . ? C1 C2 C3 C4 -5(2) . . . . ? C40 C2 C3 C4 172.7(12) . . . . ? C2 C3 C4 C5 7(2) . . . . ? C2 C3 C4 C43 -179.7(12) . . . . ? C3 C4 C5 C6 -9(2) . . . . ? C43 C4 C5 C6 178.7(12) . . . . ? C4 C5 C6 C1 7(2) . . . . ? C4 C5 C6 C37 -173.3(12) . . . . ? N1 C1 C6 C5 171.8(11) . . . . ? C2 C1 C6 C5 -4.2(19) . . . . ? N1 C1 C6 C37 -7.7(19) . . . . ? C2 C1 C6 C37 176.3(12) . . . . ? C1 N1 C7 C9 -178.5(10) . . . . ? Ni1 N1 C7 C9 3.2(13) . . . . ? C1 N1 C7 C8 4.9(18) . . . . ? Ni1 N1 C7 C8 -173.4(9) . . . . ? C13 N2 C9 C10 3.1(17) . . . . ? Ni1 N2 C9 C10 174.8(9) . . . . ? C13 N2 C9 C7 177.5(11) . . . . ? Ni1 N2 C9 C7 -10.8(13) . . . . ? N1 C7 C9 C10 177.4(13) . . . . ? C8 C7 C9 C10 -5.6(19) . . . . ? N1 C7 C9 N2 4.3(16) . . . . ? C8 C7 C9 N2 -178.8(10) . . . . ? N2 C9 C10 C11 -4(2) . . . . ? C7 C9 C10 C11 -176.8(13) . . . . ? C9 C10 C11 C12 3(2) . . . . ? C10 C11 C12 C13 -1.3(18) . . . . ? C11 C12 C13 N2 0.8(19) . . . . ? C11 C12 C13 C14 -172.3(12) . . . . ? C9 N2 C13 C12 -1.8(19) . . . . ? Ni1 N2 C13 C12 -173.2(10) . . . . ? C9 N2 C13 C14 172.4(11) . . . . ? Ni1 N2 C13 C14 0.9(14) . . . . ? C18 N3 C14 C15 1.3(18) . . . . ? Ni1 N3 C14 C15 -171.4(9) . . . . ? C18 N3 C14 C13 177.9(11) . . . . ? Ni1 N3 C14 C13 5.3(15) . . . . ? C12 C13 C14 N3 169.7(12) . . . . ? N2 C13 C14 N3 -4.3(17) . . . . ? C12 C13 C14 C15 -14(2) . . . . ? N2 C13 C14 C15 172.4(11) . . . . ? N3 C14 C15 C16 -2.2(18) . . . . ? C13 C14 C15 C16 -178.8(11) . . . . ? C14 C15 C16 C17 1.5(19) . . . . ? C15 C16 C17 C18 0(2) . . . . ? C16 C17 C18 N3 -1(2) . . . . ? C16 C17 C18 C19 -174.4(14) . . . . ? C14 N3 C18 C17 0.3(19) . . . . ? Ni1 N3 C18 C17 171.2(9) . . . . ? C14 N3 C18 C19 174.7(11) . . . . ? Ni1 N3 C18 C19 -14.4(17) . . . . ? C23 N4 C19 C20 -12.4(18) . . . . ? Ni2 N4 C19 C20 156.8(10) . . . . ? C23 N4 C19 C18 176.0(11) . . . . ? Ni2 N4 C19 C18 -14.8(17) . . . . ? C17 C18 C19 N4 116.2(15) . . . . ? N3 C18 C19 N4 -57.5(16) . . . . ? C17 C18 C19 C20 -56(2) . . . . ? N3 C18 C19 C20 130.7(13) . . . . ? N4 C19 C20 C21 11(2) . . . . ? C18 C19 C20 C21 -178.1(13) . . . . ? C19 C20 C21 C22 -1.9(19) . . . . ? C20 C21 C22 C23 -3.9(19) . . . . ? C21 C22 C23 N4 1.6(19) . . . . ? C21 C22 C23 C24 -170.6(11) . . . . ? C19 N4 C23 C22 6.5(17) . . . . ? Ni2 N4 C23 C22 -164.5(9) . . . . ? C19 N4 C23 C24 179.9(10) . . . . ? Ni2 N4 C23 C24 8.9(12) . . . . ? C28 N5 C24 C25 6.3(19) . . . . ? Ni2 N5 C24 C25 -173.0(11) . . . . ? C28 N5 C24 C23 175.7(9) . . . . ? Ni2 N5 C24 C23 -3.7(14) . . . . ? C22 C23 C24 N5 168.5(12) . . . . ? N4 C23 C24 N5 -4.3(14) . . . . ? C22 C23 C24 C25 -20.1(18) . . . . ? N4 C23 C24 C25 167.1(10) . . . . ? N5 C24 C25 C26 -7(2) . . . . ? C23 C24 C25 C26 -175.9(10) . . . . ? C24 C25 C26 C27 0.5(18) . . . . ? C25 C26 C27 C28 6(2) . . . . ? C24 N5 C28 C27 0.9(16) . . . . ? Ni2 N5 C28 C27 -179.7(10) . . . . ? C24 N5 C28 C29 176.4(11) . . . . ? Ni2 N5 C28 C29 -4.1(13) . . . . ? C26 C27 C28 N5 -7(2) . . . . ? C26 C27 C28 C29 178.5(14) . . . . ? C31 N6 C29 C28 -173.5(11) . . . . ? Ni2 N6 C29 C28 -1.3(15) . . . . ? C31 N6 C29 C30 14(2) . . . . ? Ni2 N6 C29 C30 -173.9(10) . . . . ? N5 C28 C29 N6 3.5(17) . . . . ? C27 C28 C29 N6 178.7(13) . . . . ? N5 C28 C29 C30 176.2(11) . . . . ? C27 C28 C29 C30 -9(2) . . . . ? C29 N6 C31 C36 91.1(17) . . . . ? Ni2 N6 C31 C36 -79.6(16) . . . . ? C29 N6 C31 C32 -93.4(15) . . . . ? Ni2 N6 C31 C32 95.9(12) . . . . ? N6 C31 C32 C33 -177.0(11) . . . . ? C36 C31 C32 C33 -1.1(19) . . . . ? N6 C31 C32 C52 6.5(19) . . . . ? C36 C31 C32 C52 -177.7(12) . . . . ? C31 C32 C33 C34 -1(2) . . . . ? C52 C32 C33 C34 176.1(13) . . . . ? C32 C33 C34 C35 1(2) . . . . ? C32 C33 C34 C49 173.4(14) . . . . ? C33 C34 C35 C36 2(2) . . . . ? C49 C34 C35 C36 -171.5(14) . . . . ? C34 C35 C36 C31 -4(2) . . . . ? C34 C35 C36 C46 -175.4(12) . . . . ? N6 C31 C36 C35 178.5(13) . . . . ? C32 C31 C36 C35 3(2) . . . . ? N6 C31 C36 C46 -9(2) . . . . ? C32 C31 C36 C46 175.5(12) . . . . ? C5 C6 C37 C38 87.1(15) . . . . ? C1 C6 C37 C38 -93.4(15) . . . . ? C5 C6 C37 C39 -40.7(17) . . . . ? C1 C6 C37 C39 138.8(12) . . . . ? C1 C2 C40 C41 119.3(14) . . . . ? C3 C2 C40 C41 -58.8(16) . . . . ? C1 C2 C40 C42 -124.0(13) . . . . ? C3 C2 C40 C42 57.9(15) . . . . ? C5 C4 C43 C45 -62.5(18) . . . . ? C3 C4 C43 C45 125.2(15) . . . . ? C5 C4 C43 C44 63.2(18) . . . . ? C3 C4 C43 C44 -109.1(15) . . . . ? C35 C36 C46 C48 65.8(17) . . . . ? C31 C36 C46 C48 -106.5(14) . . . . ? C35 C36 C46 C47 -52.1(16) . . . . ? C31 C36 C46 C47 135.6(12) . . . . ? C33 C34 C49 C51 145.4(18) . . . . ? C35 C34 C49 C51 -42(2) . . . . ? C33 C34 C49 C50 -78(2) . . . . ? C35 C34 C49 C50 94(2) . . . . ? C31 C32 C52 C53 116.2(15) . . . . ? C33 C32 C52 C53 -60.2(17) . . . . ? C31 C32 C52 C54 -121.6(15) . . . . ? C33 C32 C52 C54 61.9(16) . . . . ? Ni2 N7 C55 C56 51(16) . . . . ? N2A Ni2A Cl1A Ni1A 110.0(3) . . . . ? N8A Ni2A Cl1A Ni1A -82.3(3) . . . . ? N1A Ni2A Cl1A Ni1A -173.6(3) . . . . ? N3A Ni2A Cl1A Ni1A 30.4(3) . . . . ? Cl2A Ni2A Cl1A Ni1A -14.1(10) . . . . ? N7A Ni1A Cl1A Ni2A -81.0(3) . . . . ? N5A Ni1A Cl1A Ni2A 108.7(3) . . . . ? N4A Ni1A Cl1A Ni2A 32.3(3) . . . . ? N6A Ni1A Cl1A Ni2A -173.8(3) . . . . ? Cl3A Ni1A Cl1A Ni2A -17.1(11) . . . . ? N2A Ni2A N1A C7A 6.7(9) . . . . ? N8A Ni2A N1A C7A -170.8(9) . . . . ? N3A Ni2A N1A C7A 3.3(15) . . . . ? Cl2A Ni2A N1A C7A 101.1(9) . . . . ? Cl1A Ni2A N1A C7A -82.1(9) . . . . ? N2A Ni2A N1A C1A 173.2(10) . . . . ? N8A Ni2A N1A C1A -4.3(9) . . . . ? N3A Ni2A N1A C1A 169.8(9) . . . . ? Cl2A Ni2A N1A C1A -92.3(9) . . . . ? Cl1A Ni2A N1A C1A 84.4(9) . . . . ? N8A Ni2A N2A C9A 6(2) . . . . ? N1A Ni2A N2A C9A -5.9(10) . . . . ? N3A Ni2A N2A C9A 172.7(11) . . . . ? Cl2A Ni2A N2A C9A -102.5(10) . . . . ? Cl1A Ni2A N2A C9A 85.2(10) . . . . ? N8A Ni2A N2A C13A -171.6(15) . . . . ? N1A Ni2A N2A C13A 176.7(10) . . . . ? N3A Ni2A N2A C13A -4.7(9) . . . . ? Cl2A Ni2A N2A C13A 80.1(9) . . . . ? Cl1A Ni2A N2A C13A -92.2(9) . . . . ? N2A Ni2A N3A C18A -179.8(11) . . . . ? N8A Ni2A N3A C18A -2.9(12) . . . . ? N1A Ni2A N3A C18A -176.5(10) . . . . ? Cl2A Ni2A N3A C18A 83.2(11) . . . . ? Cl1A Ni2A N3A C18A -90.3(11) . . . . ? N2A Ni2A N3A C14A 9.5(9) . . . . ? N8A Ni2A N3A C14A -173.5(9) . . . . ? N1A Ni2A N3A C14A 12.8(15) . . . . ? Cl2A Ni2A N3A C14A -87.5(9) . . . . ? Cl1A Ni2A N3A C14A 99.0(9) . . . . ? N7A Ni1A N4A C19A -1.8(11) . . . . ? N5A Ni1A N4A C19A -179.0(10) . . . . ? N6A Ni1A N4A C19A -173.0(9) . . . . ? Cl3A Ni1A N4A C19A 83.4(9) . . . . ? Cl1A Ni1A N4A C19A -90.1(10) . . . . ? N7A Ni1A N4A C23A -173.1(7) . . . . ? N5A Ni1A N4A C23A 9.7(7) . . . . ? N6A Ni1A N4A C23A 15.7(13) . . . . ? Cl3A Ni1A N4A C23A -87.9(7) . . . . ? Cl1A Ni1A N4A C23A 98.6(7) . . . . ? N7A Ni1A N5A C24A -169(2) . . . . ? N4A Ni1A N5A C24A -4.5(9) . . . . ? N6A Ni1A N5A C24A 178.2(10) . . . . ? Cl3A Ni1A N5A C24A 80.9(9) . . . . ? Cl1A Ni1A N5A C24A -92.1(9) . . . . ? N7A Ni1A N5A C28A 9(3) . . . . ? N4A Ni1A N5A C28A 173.5(9) . . . . ? N6A Ni1A N5A C28A -3.7(8) . . . . ? Cl3A Ni1A N5A C28A -101.1(8) . . . . ? Cl1A Ni1A N5A C28A 85.9(8) . . . . ? N7A Ni1A N6A C29A -172.4(10) . . . . ? N5A Ni1A N6A C29A 5.5(9) . . . . ? N4A Ni1A N6A C29A -0.5(15) . . . . ? Cl3A Ni1A N6A C29A 100.5(10) . . . . ? Cl1A Ni1A N6A C29A -82.9(10) . . . . ? N7A Ni1A N6A C31A 3.9(10) . . . . ? N5A Ni1A N6A C31A -178.2(10) . . . . ? N4A Ni1A N6A C31A 175.8(8) . . . . ? Cl3A Ni1A N6A C31A -83.2(10) . . . . ? Cl1A Ni1A N6A C31A 93.4(9) . . . . ? N5A Ni1A N7A C55A -23(7) . . . . ? N4A Ni1A N7A C55A 173(6) . . . . ? N6A Ni1A N7A C55A -11(6) . . . . ? Cl3A Ni1A N7A C55A 87(6) . . . . ? Cl1A Ni1A N7A C55A -100(6) . . . . ? N2A Ni2A N8A C57A -37(4) . . . . ? N1A Ni2A N8A C57A -25(3) . . . . ? N3A Ni2A N8A C57A 157(3) . . . . ? Cl2A Ni2A N8A C57A 73(3) . . . . ? Cl1A Ni2A N8A C57A -116(3) . . . . ? C7A N1A C1A C2A 84.2(16) . . . . ? Ni2A N1A C1A C2A -82.0(15) . . . . ? C7A N1A C1A C6A -99.9(13) . . . . ? Ni2A N1A C1A C6A 93.9(12) . . . . ? C6A C1A C2A C3A -2(2) . . . . ? N1A C1A C2A C3A 174.0(11) . . . . ? C6A C1A C2A C40A 175.5(12) . . . . ? N1A C1A C2A C40A -9(2) . . . . ? C1A C2A C3A C4A -1(2) . . . . ? C40A C2A C3A C4A -178.3(12) . . . . ? C2A C3A C4A C5A 2(2) . . . . ? C2A C3A C4A C43A -176.4(14) . . . . ? C3A C4A C5A C6A 0(2) . . . . ? C43A C4A C5A C6A 178.1(14) . . . . ? C4A C5A C6A C1A -2(2) . . . . ? C4A C5A C6A C37A -178.0(13) . . . . ? C2A C1A C6A C5A 3(2) . . . . ? N1A C1A C6A C5A -173.1(11) . . . . ? C2A C1A C6A C37A 178.8(13) . . . . ? N1A C1A C6A C37A 2.6(18) . . . . ? C1A N1A C7A C9A -175.1(10) . . . . ? Ni2A N1A C7A C9A -6.7(15) . . . . ? C1A N1A C7A C8A 0.1(19) . . . . ? Ni2A N1A C7A C8A 168.4(11) . . . . ? C13A N2A C9A C10A 3(2) . . . . ? Ni2A N2A C9A C10A -173.8(9) . . . . ? C13A N2A C9A C7A -178.8(12) . . . . ? Ni2A N2A C9A C7A 4.2(15) . . . . ? N1A C7A C9A N2A 2.0(18) . . . . ? C8A C7A C9A N2A -173.8(11) . . . . ? N1A C7A C9A C10A 179.7(13) . . . . ? C8A C7A C9A C10A 4(2) . . . . ? N2A C9A C10A C11A -3(2) . . . . ? C7A C9A C10A C11A 179.0(13) . . . . ? C9A C10A C11A C12A 0(2) . . . . ? C10A C11A C12A C13A 4(2) . . . . ? C9A N2A C13A C12A 1(2) . . . . ? Ni2A N2A C13A C12A 178.0(10) . . . . ? C9A N2A C13A C14A -177.4(13) . . . . ? Ni2A N2A C13A C14A -0.2(15) . . . . ? C11A C12A C13A N2A -5(2) . . . . ? C11A C12A C13A C14A 173.5(13) . . . . ? C18A N3A C14A C15A -1(2) . . . . ? Ni2A N3A C14A C15A 170.5(11) . . . . ? C18A N3A C14A C13A 176.3(11) . . . . ? Ni2A N3A C14A C13A -12.0(15) . . . . ? N2A C13A C14A N3A 8.9(19) . . . . ? C12A C13A C14A N3A -169.1(13) . . . . ? N2A C13A C14A C15A -173.5(12) . . . . ? C12A C13A C14A C15A 8(2) . . . . ? N3A C14A C15A C16A 1(2) . . . . ? C13A C14A C15A C16A -175.9(12) . . . . ? C14A C15A C16A C17A -1(2) . . . . ? C15A C16A C17A C18A 1(2) . . . . ? C14A N3A C18A C17A 0.6(19) . . . . ? Ni2A N3A C18A C17A -169.5(9) . . . . ? C14A N3A C18A C19A -174.9(11) . . . . ? Ni2A N3A C18A C19A 15.1(16) . . . . ? C16A C17A C18A N3A 0(2) . . . . ? C16A C17A C18A C19A 174.8(11) . . . . ? C23A N4A C19A C20A 3.2(16) . . . . ? Ni1A N4A C19A C20A -167.8(8) . . . . ? C23A N4A C19A C18A -176.2(10) . . . . ? Ni1A N4A C19A C18A 12.8(15) . . . . ? N3A C18A C19A N4A 60.5(14) . . . . ? C17A C18A C19A N4A -114.9(14) . . . . ? N3A C18A C19A C20A -119.0(13) . . . . ? C17A C18A C19A C20A 65.7(15) . . . . ? N4A C19A C20A C21A -0.6(17) . . . . ? C18A C19A C20A C21A 178.8(11) . . . . ? C19A C20A C21A C22A -1.9(18) . . . . ? C20A C21A C22A C23A 2(2) . . . . ? C19A N4A C23A C22A -3.2(15) . . . . ? Ni1A N4A C23A C22A 169.4(8) . . . . ? C19A N4A C23A C24A 173.8(10) . . . . ? Ni1A N4A C23A C24A -13.6(12) . . . . ? C21A C22A C23A N4A 0.7(19) . . . . ? C21A C22A C23A C24A -176.0(12) . . . . ? C28A N5A C24A C25A 1.2(18) . . . . ? Ni1A N5A C24A C25A 179.2(9) . . . . ? C28A N5A C24A C23A -179.4(10) . . . . ? Ni1A N5A C24A C23A -1.4(14) . . . . ? N4A C23A C24A N5A 10.3(15) . . . . ? C22A C23A C24A N5A -172.8(11) . . . . ? N4A C23A C24A C25A -170.3(11) . . . . ? C22A C23A C24A C25A 7(2) . . . . ? N5A C24A C25A C26A -0.5(18) . . . . ? C23A C24A C25A C26A -179.8(11) . . . . ? C24A C25A C26A C27A 0.0(19) . . . . ? C25A C26A C27A C28A -0.3(18) . . . . ? C24A N5A C28A C27A -1.5(19) . . . . ? Ni1A N5A C28A C27A -179.6(10) . . . . ? C24A N5A C28A C29A 179.6(11) . . . . ? Ni1A N5A C28A C29A 1.6(14) . . . . ? C26A C27A C28A N5A 1.0(18) . . . . ? C26A C27A C28A C29A 179.8(11) . . . . ? C31A N6A C29A C28A 177.3(11) . . . . ? Ni1A N6A C29A C28A -6.4(15) . . . . ? C31A N6A C29A C30A 3(2) . . . . ? Ni1A N6A C29A C30A 178.9(10) . . . . ? N5A C28A C29A N6A 3.7(18) . . . . ? C27A C28A C29A N6A -175.2(12) . . . . ? N5A C28A C29A C30A 178.3(11) . . . . ? C27A C28A C29A C30A -0.6(19) . . . . ? C29A N6A C31A C36A -98.1(16) . . . . ? Ni1A N6A C31A C36A 86.1(13) . . . . ? C29A N6A C31A C32A 85.8(17) . . . . ? Ni1A N6A C31A C32A -90.1(13) . . . . ? C36A C31A C32A C33A -2(2) . . . . ? N6A C31A C32A C33A 174.0(11) . . . . ? C36A C31A C32A C49A 177.4(12) . . . . ? N6A C31A C32A C49A -7(2) . . . . ? C31A C32A C33A C34A 2(2) . . . . ? C49A C32A C33A C34A -177.6(12) . . . . ? C32A C33A C34A C35A 0(2) . . . . ? C32A C33A C34A C52A -176.9(12) . . . . ? C33A C34A C35A C36A -1(2) . . . . ? C52A C34A C35A C36A 175.5(12) . . . . ? C32A C31A C36A C35A 1(2) . . . . ? N6A C31A C36A C35A -175.4(11) . . . . ? C32A C31A C36A C46A -176.9(13) . . . . ? N6A C31A C36A C46A 7(2) . . . . ? C34A C35A C36A C31A 0.8(19) . . . . ? C34A C35A C36A C46A 178.6(12) . . . . ? C5A C6A C37A C39A 44.9(19) . . . . ? C1A C6A C37A C39A -130.5(14) . . . . ? C5A C6A C37A C38A -81.0(17) . . . . ? C1A C6A C37A C38A 103.5(15) . . . . ? C1A C2A C40A C41A -117.0(14) . . . . ? C3A C2A C40A C41A 59.9(17) . . . . ? C1A C2A C40A C42A 123.4(13) . . . . ? C3A C2A C40A C42A -59.6(16) . . . . ? C5A C4A C43A C45A 36(2) . . . . ? C3A C4A C43A C45A -145.5(15) . . . . ? C5A C4A C43A C44A -88.7(19) . . . . ? C3A C4A C43A C44A 89.6(18) . . . . ? C31A C36A C46A C47A -134.2(14) . . . . ? C35A C36A C46A C47A 48.3(17) . . . . ? C31A C36A C46A C48A 99.9(15) . . . . ? C35A C36A C46A C48A -77.5(15) . . . . ? C33A C32A C49A C50A 66.2(16) . . . . ? C31A C32A C49A C50A -112.9(15) . . . . ? C33A C32A C49A C51A -62.3(15) . . . . ? C31A C32A C49A C51A 118.5(14) . . . . ? C33A C34A C52A C53A 109.4(15) . . . . ? C35A C34A C52A C53A -67.1(17) . . . . ? C33A C34A C52A C54A -126.5(13) . . . . ? C35A C34A C52A C54A 56.9(16) . . . . ? Ni1A N7A C55A C56A -19(19) . . . . ? Ni2A N8A C57A C58A 156(15) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.485 _refine_diff_density_min -0.871 _refine_diff_density_rms 0.185 # Attachment '09011_rev.cif' data_09011 _database_code_depnum_ccdc_archive 'CCDC 745220' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C54 H68 Br3 N6 Ni2 O2)(Br)5(C H Cl3)0.5(H2 O)' _chemical_formula_sum 'C59 H74 Br4 Cl15 N6 Ni2 O2.50' _chemical_formula_weight 1876.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.709(3) _cell_length_b 16.267(3) _cell_length_c 27.122(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.154(4) _cell_angle_gamma 90.00 _cell_volume 7768(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 892 _cell_measurement_theta_min 2.504 _cell_measurement_theta_max 24.301 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3764 _exptl_absorpt_coefficient_mu 3.102 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.472 _exptl_absorpt_correction_T_max 0.694 _exptl_absorpt_process_details ; absorption correction based on 11080 reflections(SADABS);Rint 0.1658 before correction and 0.0446 after. ; _exptl_special_details ; The data was weak due to crystal quality. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59875 _diffrn_reflns_av_R_equivalents 0.1337 _diffrn_reflns_av_sigmaI/netI 0.1487 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15230 _reflns_number_gt 7864 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The methyl carbon atoms and the solvent molecules are disordered,attempts to split the atoms failed. The hydrogen atoms of the H2O molecules have been omitted from the model but have been included in all formulae Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15230 _refine_ls_number_parameters 825 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1344 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1345 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.25914(4) -0.16250(5) 0.07606(3) 0.0260(2) Uani 1 1 d . . . Ni2 Ni 0.24661(4) 0.14327(5) -0.00368(3) 0.0275(2) Uani 1 1 d . . . Br1 Br 0.24980(5) -0.29223(5) 0.02450(3) 0.0540(2) Uani 1 1 d . . . Br2 Br 0.35493(3) 0.09907(4) 0.05285(2) 0.02733(16) Uani 1 1 d . . . Br3 Br 0.30947(4) 0.17928(4) -0.07931(2) 0.03125(17) Uani 1 1 d . . . O1 O 0.1437(2) -0.1467(4) 0.05859(17) 0.0655(17) Uani 1 1 d . . . O2 O 0.2587(2) -0.0433(2) 0.10558(15) 0.0329(11) Uani 1 1 d . . . N1 N 0.2468(3) -0.2219(3) 0.14831(17) 0.0238(12) Uani 1 1 d . . . N2 N 0.3656(3) -0.1825(3) 0.10372(18) 0.0258(12) Uani 1 1 d . . . N3 N 0.3242(3) -0.1064(3) 0.01909(17) 0.0243(12) Uani 1 1 d . . . N4 N 0.1993(3) 0.0325(3) -0.04125(16) 0.0234(12) Uani 1 1 d . . . N5 N 0.1508(3) 0.1860(3) -0.03798(17) 0.0245(12) Uani 1 1 d . . . N6 N 0.2458(3) 0.2685(3) 0.02266(18) 0.0272(12) Uani 1 1 d . . . C1 C 0.1787(3) -0.2435(4) 0.1713(2) 0.0263(15) Uani 1 1 d . . . C2 C 0.1511(3) -0.3236(4) 0.1681(2) 0.0281(15) Uani 1 1 d . . . C3 C 0.0900(4) -0.3426(4) 0.1948(2) 0.0379(18) Uani 1 1 d . . . H3 H 0.0705 -0.3971 0.1933 0.045 Uiso 1 1 calc R . . C4 C 0.0568(4) -0.2848(5) 0.2236(2) 0.0399(18) Uani 1 1 d . . . C5 C 0.0854(4) -0.2068(5) 0.2252(2) 0.0402(18) Uani 1 1 d . . . H5 H 0.0631 -0.1667 0.2445 0.048 Uiso 1 1 calc R . . C6 C 0.1460(4) -0.1839(4) 0.1995(2) 0.0295(16) Uani 1 1 d . . . C7 C 0.1832(4) -0.3889(4) 0.1365(3) 0.0376(17) Uani 1 1 d . . . H7 H 0.2269 -0.3643 0.1213 0.045 Uiso 1 1 calc R . . C8 C 0.2133(4) -0.4631(5) 0.1683(3) 0.067(3) Uani 1 1 d . . . H8A H 0.2500 -0.4439 0.1955 0.100 Uiso 1 1 calc R . . H8B H 0.2381 -0.5019 0.1476 0.100 Uiso 1 1 calc R . . H8C H 0.1709 -0.4905 0.1820 0.100 Uiso 1 1 calc R . . C9 C 0.1240(4) -0.4159(4) 0.0945(3) 0.053(2) Uani 1 1 d . . . H9A H 0.0799 -0.4393 0.1085 0.079 Uiso 1 1 calc R . . H9B H 0.1461 -0.4575 0.0742 0.079 Uiso 1 1 calc R . . H9C H 0.1079 -0.3683 0.0738 0.079 Uiso 1 1 calc R . . C10 C 0.1762(4) -0.0964(4) 0.2052(2) 0.0398(18) Uani 1 1 d . . . H10 H 0.2159 -0.0902 0.1819 0.048 Uiso 1 1 calc R . . C11 C 0.1147(5) -0.0331(5) 0.1903(3) 0.079(3) Uani 1 1 d . . . H11A H 0.0963 -0.0401 0.1552 0.119 Uiso 1 1 calc R . . H11B H 0.1358 0.0223 0.1958 0.119 Uiso 1 1 calc R . . H11C H 0.0725 -0.0407 0.2105 0.119 Uiso 1 1 calc R . . C12 C 0.2145(5) -0.0797(5) 0.2572(3) 0.083(3) Uani 1 1 d . . . H12A H 0.1783 -0.0897 0.2814 0.125 Uiso 1 1 calc R . . H12B H 0.2315 -0.0224 0.2595 0.125 Uiso 1 1 calc R . . H12C H 0.2583 -0.1163 0.2641 0.125 Uiso 1 1 calc R . . C13 C -0.0080(4) -0.3093(5) 0.2531(3) 0.052(2) Uani 1 1 d . . . H13 H -0.0290 -0.2565 0.2646 0.063 Uiso 1 1 calc R . . C14 C -0.0722(5) -0.3500(7) 0.2232(3) 0.115(4) Uani 1 1 d . . . H14A H -0.0859 -0.3184 0.1927 0.173 Uiso 1 1 calc R . . H14B H -0.1160 -0.3526 0.2424 0.173 Uiso 1 1 calc R . . H14C H -0.0573 -0.4058 0.2146 0.173 Uiso 1 1 calc R . . C15 C 0.0218(4) -0.3547(6) 0.2996(3) 0.069(3) Uani 1 1 d . . . H15A H -0.0195 -0.3631 0.3204 0.104 Uiso 1 1 calc R . . H15B H 0.0623 -0.3224 0.3179 0.104 Uiso 1 1 calc R . . H15C H 0.0421 -0.4081 0.2907 0.104 Uiso 1 1 calc R . . C16 C 0.3226(4) -0.2774(4) 0.2231(2) 0.0445(19) Uani 1 1 d . . . H16A H 0.3533 -0.2407 0.2458 0.067 Uiso 1 1 calc R . . H16B H 0.3490 -0.3300 0.2210 0.067 Uiso 1 1 calc R . . H16C H 0.2733 -0.2866 0.2355 0.067 Uiso 1 1 calc R . . C17 C 0.3107(3) -0.2389(4) 0.1727(2) 0.0266(15) Uani 1 1 d . . . C18 C 0.3788(3) -0.2178(4) 0.1485(2) 0.0291(16) Uani 1 1 d . . . C19 C 0.4533(4) -0.2329(4) 0.1693(2) 0.0401(18) Uani 1 1 d . . . H19 H 0.4629 -0.2588 0.2007 0.048 Uiso 1 1 calc R . . C20 C 0.5127(4) -0.2093(5) 0.1434(3) 0.046(2) Uani 1 1 d . . . H20 H 0.5637 -0.2181 0.1570 0.055 Uiso 1 1 calc R . . C21 C 0.4973(3) -0.1730(4) 0.0976(2) 0.0374(17) Uani 1 1 d . . . H21 H 0.5379 -0.1565 0.0796 0.045 Uiso 1 1 calc R . . C22 C 0.4229(3) -0.1606(4) 0.0778(2) 0.0274(15) Uani 1 1 d . . . C23 C 0.3999(3) -0.1205(4) 0.0300(2) 0.0271(15) Uani 1 1 d . . . C24 C 0.4528(4) -0.0965(4) -0.0011(2) 0.0301(16) Uani 1 1 d . . . H24 H 0.5050 -0.1092 0.0072 0.036 Uiso 1 1 calc R . . C25 C 0.4301(4) -0.0544(4) -0.0437(2) 0.0299(16) Uani 1 1 d . . . H25 H 0.4658 -0.0388 -0.0657 0.036 Uiso 1 1 calc R . . C26 C 0.3543(4) -0.0351(4) -0.0539(2) 0.0294(16) Uani 1 1 d . . . H26 H 0.3373 -0.0034 -0.0824 0.035 Uiso 1 1 calc R . . C27 C 0.3031(3) -0.0627(4) -0.0222(2) 0.0238(14) Uani 1 1 d . . . C28 C 0.2220(3) -0.0468(4) -0.0376(2) 0.0243(15) Uani 1 1 d . . . C29 C 0.1739(4) -0.1110(4) -0.0539(2) 0.0318(16) Uani 1 1 d . . . H29 H 0.1903 -0.1664 -0.0496 0.038 Uiso 1 1 calc R . . C30 C 0.1023(4) -0.0936(4) -0.0763(2) 0.0385(18) Uani 1 1 d . . . H30 H 0.0685 -0.1369 -0.0869 0.046 Uiso 1 1 calc R . . C31 C 0.0803(4) -0.0138(4) -0.0830(2) 0.0352(17) Uani 1 1 d . . . H31 H 0.0323 -0.0006 -0.1004 0.042 Uiso 1 1 calc R . . C32 C 0.1292(3) 0.0478(4) -0.0641(2) 0.0265(15) Uani 1 1 d . . . C33 C 0.1062(3) 0.1357(4) -0.0673(2) 0.0269(15) Uani 1 1 d . . . C34 C 0.0444(4) 0.1673(5) -0.0968(2) 0.0374(18) Uani 1 1 d . . . H34 H 0.0122 0.1321 -0.1177 0.045 Uiso 1 1 calc R . . C35 C 0.0303(4) 0.2505(4) -0.0954(2) 0.0399(18) Uani 1 1 d . . . H35 H -0.0120 0.2728 -0.1155 0.048 Uiso 1 1 calc R . . C36 C 0.0765(4) 0.3015(4) -0.0653(2) 0.0346(17) Uani 1 1 d . . . H36 H 0.0671 0.3590 -0.0645 0.042 Uiso 1 1 calc R . . C37 C 0.1377(3) 0.2668(4) -0.0359(2) 0.0269(15) Uani 1 1 d . . . C38 C 0.1916(4) 0.3110(4) -0.0001(2) 0.0317(16) Uani 1 1 d . . . C39 C 0.1775(4) 0.4008(4) 0.0078(2) 0.0432(19) Uani 1 1 d . . . H39A H 0.2118 0.4207 0.0360 0.065 Uiso 1 1 calc R . . H39B H 0.1247 0.4088 0.0146 0.065 Uiso 1 1 calc R . . H39C H 0.1866 0.4315 -0.0221 0.065 Uiso 1 1 calc R . . C40 C 0.2976(4) 0.3081(4) 0.0597(2) 0.0318(16) Uani 1 1 d . . . C41 C 0.2874(4) 0.2944(4) 0.1096(2) 0.0397(18) Uani 1 1 d . . . C42 C 0.3381(5) 0.3303(5) 0.1457(3) 0.053(2) Uani 1 1 d . . . H42 H 0.3311 0.3217 0.1795 0.063 Uiso 1 1 calc R . . C43 C 0.3988(5) 0.3785(5) 0.1344(3) 0.059(2) Uani 1 1 d . . . C44 C 0.4075(4) 0.3896(4) 0.0849(3) 0.049(2) Uani 1 1 d . . . H44 H 0.4489 0.4221 0.0765 0.059 Uiso 1 1 calc R . . C45 C 0.3589(4) 0.3557(4) 0.0468(3) 0.0373(17) Uani 1 1 d . . . C46 C 0.2198(5) 0.2458(5) 0.1235(3) 0.054(2) Uani 1 1 d . . . H46 H 0.1998 0.2133 0.0936 0.065 Uiso 1 1 calc R . . C47 C 0.1560(5) 0.3045(6) 0.1355(4) 0.095(3) Uani 1 1 d . . . H47A H 0.1726 0.3352 0.1658 0.142 Uiso 1 1 calc R . . H47B H 0.1105 0.2726 0.1405 0.142 Uiso 1 1 calc R . . H47C H 0.1443 0.3430 0.1080 0.142 Uiso 1 1 calc R . . C48 C 0.2395(5) 0.1858(5) 0.1649(3) 0.071(3) Uani 1 1 d . . . H48A H 0.2824 0.1517 0.1573 0.107 Uiso 1 1 calc R . . H48B H 0.1956 0.1506 0.1687 0.107 Uiso 1 1 calc R . . H48C H 0.2535 0.2159 0.1959 0.107 Uiso 1 1 calc R . . C49 C 0.4525(6) 0.4179(6) 0.1755(4) 0.097(4) Uani 1 1 d . . . H49 H 0.4909 0.4310 0.1521 0.117 Uiso 1 1 calc R . . C50 C 0.5004(8) 0.3740(7) 0.2032(5) 0.190(8) Uani 1 1 d . . . H50A H 0.5307 0.4096 0.2269 0.285 Uiso 1 1 calc R . . H50B H 0.5340 0.3452 0.1826 0.285 Uiso 1 1 calc R . . H50C H 0.4729 0.3337 0.2214 0.285 Uiso 1 1 calc R . . C51 C 0.4340(5) 0.5038(5) 0.1812(3) 0.080(3) Uani 1 1 d . . . H51A H 0.3847 0.5084 0.1943 0.121 Uiso 1 1 calc R . . H51B H 0.4314 0.5312 0.1489 0.121 Uiso 1 1 calc R . . H51C H 0.4732 0.5299 0.2042 0.121 Uiso 1 1 calc R . . C52 C 0.3726(4) 0.3735(4) -0.0060(3) 0.045(2) Uani 1 1 d . . . H52 H 0.3300 0.3487 -0.0283 0.055 Uiso 1 1 calc R . . C53 C 0.4473(4) 0.3332(5) -0.0181(3) 0.062(2) Uani 1 1 d . . . H53A H 0.4901 0.3583 0.0023 0.093 Uiso 1 1 calc R . . H53B H 0.4533 0.3415 -0.0532 0.093 Uiso 1 1 calc R . . H53C H 0.4458 0.2742 -0.0110 0.093 Uiso 1 1 calc R . . C54 C 0.3740(5) 0.4662(5) -0.0166(3) 0.070(3) Uani 1 1 d . . . H54A H 0.3258 0.4909 -0.0096 0.105 Uiso 1 1 calc R . . H54B H 0.3813 0.4752 -0.0515 0.105 Uiso 1 1 calc R . . H54C H 0.4159 0.4918 0.0045 0.105 Uiso 1 1 calc R . . Br4 Br 0.12101(5) 0.07088(7) 0.06157(3) 0.0759(3) Uani 1 1 d . . . C55 C 0.5390(5) 0.9152(6) 0.8247(3) 0.086(3) Uani 1 1 d . . . H55 H 0.5537 0.8909 0.8582 0.104 Uiso 1 1 calc R A 1 Cl1 Cl 0.5852(3) 1.00245(19) 0.81751(14) 0.198(2) Uani 1 1 d . B . Cl2 Cl 0.5538(2) 0.84782(19) 0.77915(11) 0.1360(14) Uani 1 1 d . B . Cl3A Cl 0.4467(4) 0.9664(4) 0.8219(2) 0.101(2) Uani 0.50 1 d P B 1 Cl3B Cl 0.4454(4) 0.8897(7) 0.8237(3) 0.160(4) Uani 0.50 1 d P B 2 C56 C 0.3317(7) 0.7242(6) 0.9026(3) 0.108(4) Uani 1 1 d . . . H56 H 0.3120 0.7356 0.9351 0.129 Uiso 1 1 calc R . . Cl4 Cl 0.28531(17) 0.78728(16) 0.85890(9) 0.0953(9) Uani 1 1 d . . . Cl5 Cl 0.4294(3) 0.7418(2) 0.90929(15) 0.188(2) Uani 1 1 d . . . Cl6 Cl 0.3133(2) 0.62043(17) 0.88723(12) 0.1471(14) Uani 1 1 d . . . C57 C 0.3023(5) 0.3663(5) 0.8528(3) 0.068(3) Uani 1 1 d . . . H57 H 0.3178 0.3272 0.8805 0.082 Uiso 1 1 calc R . . Cl7 Cl 0.22504(13) 0.42712(15) 0.87047(8) 0.0768(7) Uani 1 1 d . . . Cl8 Cl 0.37929(15) 0.42696(16) 0.84440(10) 0.0908(8) Uani 1 1 d . . . Cl9 Cl 0.27473(17) 0.30918(17) 0.80046(9) 0.1001(9) Uani 1 1 d . . . C58 C 0.2200(4) 0.0788(5) 0.8110(3) 0.052(2) Uani 1 1 d . . . H58 H 0.2329 0.1109 0.8422 0.062 Uiso 1 1 calc R . . Cl10 Cl 0.12958(15) 0.10806(18) 0.78472(10) 0.1045(10) Uani 1 1 d . . . Cl11 Cl 0.28762(16) 0.09910(16) 0.77105(9) 0.0966(9) Uani 1 1 d . . . Cl12 Cl 0.22003(14) -0.02480(14) 0.82552(8) 0.0743(7) Uani 1 1 d . . . C59 C 0.0821(5) 0.6415(5) 0.9422(4) 0.084(3) Uani 1 1 d . . . H59 H 0.1301 0.6410 0.9652 0.101 Uiso 1 1 calc R . . Cl13 Cl 0.02405(16) 0.71708(18) 0.96206(10) 0.0995(9) Uani 1 1 d . . . Cl14 Cl 0.1049(2) 0.6688(3) 0.88397(14) 0.1614(15) Uani 1 1 d . . . Cl15 Cl 0.03988(19) 0.54944(17) 0.94635(18) 0.191(2) Uani 1 1 d . . . O3 O 0.0391(8) 0.9318(9) 0.0245(5) 0.109(5) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0196(4) 0.0318(5) 0.0264(4) 0.0037(4) 0.0016(3) -0.0013(4) Ni2 0.0251(5) 0.0275(5) 0.0284(5) -0.0025(4) -0.0045(4) 0.0048(4) Br1 0.0820(6) 0.0404(5) 0.0361(4) 0.0013(4) -0.0091(4) -0.0207(4) Br2 0.0228(3) 0.0309(4) 0.0275(3) -0.0014(3) -0.0010(3) 0.0017(3) Br3 0.0262(4) 0.0351(4) 0.0332(4) -0.0003(3) 0.0071(3) -0.0020(3) O1 0.018(3) 0.129(5) 0.049(3) 0.032(3) 0.005(2) -0.004(3) O2 0.040(3) 0.026(3) 0.036(3) 0.001(2) 0.017(2) 0.009(2) N1 0.023(3) 0.024(3) 0.024(3) -0.002(2) 0.000(2) 0.001(2) N2 0.025(3) 0.025(3) 0.028(3) -0.001(2) 0.004(2) 0.003(2) N3 0.020(3) 0.026(3) 0.027(3) -0.002(2) 0.005(2) 0.000(2) N4 0.021(3) 0.028(3) 0.021(3) -0.002(2) 0.002(2) -0.003(2) N5 0.022(3) 0.029(3) 0.024(3) -0.003(2) 0.005(2) -0.004(2) N6 0.027(3) 0.027(3) 0.027(3) -0.003(2) 0.001(2) 0.003(3) C1 0.020(3) 0.034(4) 0.025(4) 0.008(3) 0.002(3) -0.002(3) C2 0.026(4) 0.025(4) 0.031(4) 0.007(3) -0.003(3) 0.003(3) C3 0.031(4) 0.039(5) 0.041(4) 0.015(4) -0.012(3) -0.012(4) C4 0.034(4) 0.049(5) 0.039(4) 0.019(4) 0.011(3) 0.003(4) C5 0.040(4) 0.046(5) 0.036(4) 0.005(4) 0.008(3) 0.002(4) C6 0.032(4) 0.031(4) 0.026(4) 0.005(3) 0.004(3) -0.002(3) C7 0.029(4) 0.024(4) 0.058(5) 0.006(4) 0.002(4) -0.006(3) C8 0.061(6) 0.036(5) 0.103(7) 0.015(5) 0.010(5) 0.014(4) C9 0.048(5) 0.040(5) 0.070(6) -0.015(4) 0.009(4) -0.006(4) C10 0.050(5) 0.039(5) 0.033(4) -0.005(3) 0.019(4) -0.007(4) C11 0.070(7) 0.039(6) 0.125(8) 0.005(5) 0.001(6) -0.005(5) C12 0.100(8) 0.087(8) 0.061(6) -0.016(5) 0.001(6) -0.033(6) C13 0.033(4) 0.076(6) 0.049(5) 0.023(4) 0.010(4) -0.008(4) C14 0.055(6) 0.214(13) 0.077(7) 0.031(8) 0.008(5) -0.063(8) C15 0.051(5) 0.101(8) 0.058(6) 0.030(5) 0.014(4) -0.018(5) C16 0.032(4) 0.061(5) 0.040(4) 0.015(4) -0.002(3) -0.003(4) C17 0.026(4) 0.027(4) 0.027(4) 0.002(3) 0.004(3) -0.007(3) C18 0.024(4) 0.032(4) 0.031(4) -0.004(3) 0.000(3) 0.004(3) C19 0.029(4) 0.057(5) 0.032(4) 0.010(4) -0.007(3) 0.008(4) C20 0.022(4) 0.064(6) 0.052(5) 0.008(4) 0.003(4) 0.006(4) C21 0.018(4) 0.045(5) 0.049(5) 0.008(4) 0.007(3) 0.007(3) C22 0.023(3) 0.025(4) 0.035(4) -0.008(3) 0.006(3) 0.001(3) C23 0.026(4) 0.024(4) 0.032(4) -0.005(3) 0.006(3) 0.000(3) C24 0.024(4) 0.029(4) 0.038(4) -0.006(3) 0.008(3) 0.002(3) C25 0.030(4) 0.032(4) 0.031(4) -0.007(3) 0.019(3) -0.007(3) C26 0.034(4) 0.031(4) 0.025(4) -0.006(3) 0.010(3) -0.002(3) C27 0.029(4) 0.018(4) 0.025(4) -0.007(3) 0.006(3) 0.000(3) C28 0.032(4) 0.027(4) 0.016(3) -0.001(3) 0.008(3) -0.003(3) C29 0.038(4) 0.031(4) 0.026(4) 0.000(3) 0.002(3) -0.003(3) C30 0.044(4) 0.031(4) 0.037(4) 0.006(3) -0.013(3) -0.017(4) C31 0.028(4) 0.038(5) 0.037(4) 0.011(3) -0.008(3) -0.007(3) C32 0.022(4) 0.027(4) 0.031(4) 0.003(3) 0.002(3) -0.003(3) C33 0.019(3) 0.035(4) 0.026(4) 0.003(3) 0.002(3) 0.000(3) C34 0.026(4) 0.051(5) 0.034(4) -0.002(4) -0.001(3) 0.002(4) C35 0.030(4) 0.046(5) 0.041(4) 0.000(4) -0.007(3) 0.014(4) C36 0.035(4) 0.033(4) 0.035(4) 0.001(3) 0.001(3) 0.005(3) C37 0.025(4) 0.029(4) 0.027(4) -0.001(3) 0.004(3) 0.005(3) C38 0.033(4) 0.030(4) 0.034(4) -0.005(3) 0.010(3) 0.000(3) C39 0.043(4) 0.038(5) 0.046(4) -0.011(4) -0.005(4) 0.010(4) C40 0.029(4) 0.022(4) 0.042(4) -0.008(3) -0.001(3) 0.007(3) C41 0.041(4) 0.042(5) 0.035(4) -0.003(3) -0.004(4) 0.006(4) C42 0.062(6) 0.061(6) 0.032(4) -0.019(4) -0.006(4) 0.013(5) C43 0.053(6) 0.055(6) 0.064(6) -0.025(5) -0.022(5) 0.005(5) C44 0.032(4) 0.040(5) 0.073(6) -0.019(4) -0.001(4) -0.004(4) C45 0.031(4) 0.032(4) 0.048(5) -0.010(4) -0.001(3) 0.008(3) C46 0.066(6) 0.064(6) 0.031(4) 0.002(4) -0.002(4) -0.009(5) C47 0.059(6) 0.106(9) 0.124(9) 0.041(7) 0.036(6) 0.013(6) C48 0.077(6) 0.092(7) 0.043(5) 0.010(5) 0.003(5) -0.006(6) C49 0.082(7) 0.083(8) 0.114(9) -0.058(7) -0.051(6) 0.012(6) C50 0.229(16) 0.096(10) 0.202(14) -0.042(9) -0.178(13) 0.035(10) C51 0.054(6) 0.082(8) 0.101(8) -0.051(6) -0.009(5) -0.006(5) C52 0.043(5) 0.042(5) 0.052(5) -0.005(4) 0.005(4) -0.013(4) C53 0.050(5) 0.075(6) 0.064(6) -0.020(5) 0.018(4) -0.014(5) C54 0.074(6) 0.051(6) 0.084(7) 0.011(5) 0.008(5) -0.011(5) Br4 0.0661(6) 0.1242(9) 0.0361(5) -0.0070(5) -0.0002(4) 0.0517(6) C55 0.097(8) 0.129(10) 0.027(5) 0.015(5) -0.022(5) -0.021(7) Cl1 0.311(6) 0.074(2) 0.168(3) 0.036(2) -0.164(3) -0.055(3) Cl2 0.169(3) 0.110(2) 0.110(2) -0.0435(19) -0.075(2) 0.055(2) Cl3A 0.133(6) 0.123(5) 0.048(3) 0.011(4) 0.011(3) 0.054(5) Cl3B 0.092(5) 0.306(12) 0.085(5) -0.051(7) 0.024(4) -0.070(8) C56 0.185(13) 0.080(8) 0.056(6) -0.002(5) 0.009(7) 0.065(8) Cl4 0.142(2) 0.0759(18) 0.0691(16) 0.0129(14) 0.0138(16) 0.0458(17) Cl5 0.211(4) 0.140(3) 0.186(4) -0.083(3) -0.099(3) 0.077(3) Cl6 0.246(4) 0.057(2) 0.131(3) 0.0004(18) -0.010(3) 0.038(2) C57 0.099(7) 0.043(5) 0.059(6) -0.007(4) -0.001(5) 0.009(5) Cl7 0.0758(16) 0.0860(19) 0.0687(15) 0.0045(13) 0.0079(13) -0.0074(14) Cl8 0.0915(19) 0.085(2) 0.100(2) 0.0014(15) 0.0299(16) -0.0114(16) Cl9 0.134(2) 0.097(2) 0.0654(16) -0.0168(14) -0.0064(16) -0.0124(19) C58 0.056(5) 0.063(6) 0.035(4) -0.008(4) -0.002(4) -0.003(4) Cl10 0.092(2) 0.119(2) 0.096(2) -0.0085(17) -0.0212(16) 0.0397(18) Cl11 0.125(2) 0.0833(19) 0.0927(19) -0.0228(15) 0.0611(17) -0.0428(17) Cl12 0.1008(19) 0.0596(16) 0.0627(14) 0.0134(12) 0.0101(13) -0.0063(14) C59 0.077(7) 0.062(7) 0.104(8) 0.000(6) -0.036(6) -0.010(6) Cl13 0.096(2) 0.098(2) 0.111(2) -0.0087(17) 0.0395(18) -0.0306(18) Cl14 0.176(4) 0.194(4) 0.125(3) -0.038(3) 0.064(3) 0.006(3) Cl15 0.124(3) 0.0455(18) 0.373(6) 0.039(3) -0.120(3) -0.0266(18) O3 0.106(11) 0.126(13) 0.099(10) 0.012(9) 0.023(9) 0.008(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.980(5) . ? Ni1 O1 2.064(4) . ? Ni1 O2 2.098(4) . ? Ni1 N1 2.216(5) . ? Ni1 N3 2.220(5) . ? Ni1 Br1 2.5272(12) . ? Ni2 N5 1.972(5) . ? Ni2 N6 2.159(5) . ? Ni2 N4 2.192(5) . ? Ni2 Br2 2.4323(10) . ? Ni2 Br3 2.5060(11) . ? N1 C17 1.278(7) . ? N1 C1 1.459(7) . ? N2 C18 1.340(7) . ? N2 C22 1.344(7) . ? N3 C27 1.345(7) . ? N3 C23 1.361(7) . ? N4 C32 1.350(7) . ? N4 C28 1.352(7) . ? N5 C37 1.337(7) . ? N5 C33 1.338(7) . ? N6 C38 1.286(7) . ? N6 C40 1.439(7) . ? C1 C2 1.390(8) . ? C1 C6 1.399(8) . ? C2 C3 1.401(8) . ? C2 C7 1.514(8) . ? C3 C4 1.391(9) . ? C3 H3 0.9500 . ? C4 C5 1.366(9) . ? C4 C13 1.521(9) . ? C5 C6 1.390(8) . ? C5 H5 0.9500 . ? C6 C10 1.522(9) . ? C7 C9 1.528(9) . ? C7 C8 1.544(9) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.521(10) . ? C10 C12 1.523(9) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.479(10) . ? C13 C15 1.508(9) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.498(8) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.475(8) . ? C18 C19 1.400(8) . ? C19 C20 1.380(9) . ? C19 H19 0.9500 . ? C20 C21 1.375(9) . ? C20 H20 0.9500 . ? C21 C22 1.383(8) . ? C21 H21 0.9500 . ? C22 C23 1.468(8) . ? C23 C24 1.383(8) . ? C24 C25 1.366(8) . ? C24 H24 0.9500 . ? C25 C26 1.377(8) . ? C25 H25 0.9500 . ? C26 C27 1.390(8) . ? C26 H26 0.9500 . ? C27 C28 1.476(8) . ? C28 C29 1.390(8) . ? C29 C30 1.375(8) . ? C29 H29 0.9500 . ? C30 C31 1.362(9) . ? C30 H30 0.9500 . ? C31 C32 1.387(8) . ? C31 H31 0.9500 . ? C32 C33 1.488(8) . ? C33 C34 1.383(8) . ? C34 C35 1.379(9) . ? C34 H34 0.9500 . ? C35 C36 1.371(9) . ? C35 H35 0.9500 . ? C36 C37 1.394(8) . ? C36 H36 0.9500 . ? C37 C38 1.475(8) . ? C38 C39 1.502(8) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.403(9) . ? C40 C45 1.407(9) . ? C41 C42 1.383(9) . ? C41 C46 1.515(10) . ? C42 C43 1.391(10) . ? C42 H42 0.9500 . ? C43 C44 1.379(10) . ? C43 C49 1.527(10) . ? C44 C45 1.387(9) . ? C44 H44 0.9500 . ? C45 C52 1.508(9) . ? C46 C48 1.502(10) . ? C46 C47 1.540(11) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.288(12) . ? C49 C51 1.447(11) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C54 1.537(10) . ? C52 C53 1.542(9) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 Cl1 1.660(10) . ? C55 Cl2 1.692(9) . ? C55 Cl3B 1.706(11) . ? C55 Cl3A 1.829(11) . ? C55 H55 1.0000 . ? C56 Cl4 1.709(9) . ? C56 Cl5 1.743(13) . ? C56 Cl6 1.761(10) . ? C56 H56 1.0000 . ? C57 Cl8 1.718(9) . ? C57 Cl9 1.723(8) . ? C57 Cl7 1.795(8) . ? C57 H57 1.0000 . ? C58 Cl11 1.730(7) . ? C58 Cl12 1.731(8) . ? C58 Cl10 1.747(7) . ? C58 H58 1.0000 . ? C59 Cl15 1.683(9) . ? C59 Cl13 1.726(10) . ? C59 Cl14 1.729(10) . ? C59 H59 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 O1 170.67(19) . . ? N2 Ni1 O2 92.84(18) . . ? O1 Ni1 O2 85.9(2) . . ? N2 Ni1 N1 76.94(19) . . ? O1 Ni1 N1 93.89(18) . . ? O2 Ni1 N1 93.47(16) . . ? N2 Ni1 N3 77.71(19) . . ? O1 Ni1 N3 111.34(18) . . ? O2 Ni1 N3 84.76(16) . . ? N1 Ni1 N3 154.47(18) . . ? N2 Ni1 Br1 94.33(14) . . ? O1 Ni1 Br1 88.42(17) . . ? O2 Ni1 Br1 168.57(12) . . ? N1 Ni1 Br1 96.81(12) . . ? N3 Ni1 Br1 88.08(13) . . ? N5 Ni2 N6 77.8(2) . . ? N5 Ni2 N4 78.7(2) . . ? N6 Ni2 N4 156.01(19) . . ? N5 Ni2 Br2 169.12(14) . . ? N6 Ni2 Br2 95.92(14) . . ? N4 Ni2 Br2 106.64(13) . . ? N5 Ni2 Br3 88.10(13) . . ? N6 Ni2 Br3 94.00(13) . . ? N4 Ni2 Br3 89.58(12) . . ? Br2 Ni2 Br3 101.28(4) . . ? C17 N1 C1 117.0(5) . . ? C17 N1 Ni1 112.7(4) . . ? C1 N1 Ni1 130.3(4) . . ? C18 N2 C22 121.3(5) . . ? C18 N2 Ni1 118.6(4) . . ? C22 N2 Ni1 120.0(4) . . ? C27 N3 C23 116.7(5) . . ? C27 N3 Ni1 132.7(4) . . ? C23 N3 Ni1 110.5(4) . . ? C32 N4 C28 117.4(5) . . ? C32 N4 Ni2 110.4(4) . . ? C28 N4 Ni2 130.9(4) . . ? C37 N5 C33 122.1(5) . . ? C37 N5 Ni2 118.1(4) . . ? C33 N5 Ni2 119.3(4) . . ? C38 N6 C40 118.8(5) . . ? C38 N6 Ni2 112.3(4) . . ? C40 N6 Ni2 128.9(4) . . ? C2 C1 C6 121.4(6) . . ? C2 C1 N1 120.0(6) . . ? C6 C1 N1 118.4(6) . . ? C1 C2 C3 117.4(6) . . ? C1 C2 C7 122.9(6) . . ? C3 C2 C7 119.7(6) . . ? C4 C3 C2 122.5(6) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C5 C4 C3 117.9(6) . . ? C5 C4 C13 121.7(7) . . ? C3 C4 C13 120.4(7) . . ? C4 C5 C6 122.5(7) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 118.3(6) . . ? C5 C6 C10 118.8(6) . . ? C1 C6 C10 122.8(6) . . ? C2 C7 C9 110.8(5) . . ? C2 C7 C8 111.1(6) . . ? C9 C7 C8 111.1(6) . . ? C2 C7 H7 107.9 . . ? C9 C7 H7 107.9 . . ? C8 C7 H7 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C6 111.9(6) . . ? C11 C10 C12 111.1(7) . . ? C6 C10 C12 112.1(6) . . ? C11 C10 H10 107.1 . . ? C6 C10 H10 107.1 . . ? C12 C10 H10 107.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 114.8(7) . . ? C14 C13 C4 114.1(6) . . ? C15 C13 C4 110.6(6) . . ? C14 C13 H13 105.5 . . ? C15 C13 H13 105.5 . . ? C4 C13 H13 105.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C18 116.1(5) . . ? N1 C17 C16 126.4(6) . . ? C18 C17 C16 117.5(6) . . ? N2 C18 C19 120.3(6) . . ? N2 C18 C17 115.6(5) . . ? C19 C18 C17 124.1(6) . . ? C20 C19 C18 118.9(6) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C21 C20 C19 119.4(6) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C22 120.1(6) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? N2 C22 C21 119.9(6) . . ? N2 C22 C23 115.2(5) . . ? C21 C22 C23 124.8(6) . . ? N3 C23 C24 122.4(6) . . ? N3 C23 C22 116.2(5) . . ? C24 C23 C22 121.4(6) . . ? C25 C24 C23 120.0(6) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 118.5(6) . . ? C24 C25 H25 120.7 . . ? C26 C25 H25 120.7 . . ? C25 C26 C27 119.2(6) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? N3 C27 C26 123.0(6) . . ? N3 C27 C28 120.2(5) . . ? C26 C27 C28 116.6(5) . . ? N4 C28 C29 121.8(6) . . ? N4 C28 C27 117.4(5) . . ? C29 C28 C27 120.3(6) . . ? C30 C29 C28 119.4(6) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C31 C30 C29 119.5(6) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 118.7(6) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? N4 C32 C31 123.0(6) . . ? N4 C32 C33 115.9(5) . . ? C31 C32 C33 121.1(6) . . ? N5 C33 C34 119.8(6) . . ? N5 C33 C32 114.3(5) . . ? C34 C33 C32 125.8(6) . . ? C35 C34 C33 118.9(6) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C36 C35 C34 120.9(6) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C37 118.2(6) . . ? C35 C36 H36 120.9 . . ? C37 C36 H36 120.9 . . ? N5 C37 C36 120.2(6) . . ? N5 C37 C38 113.8(5) . . ? C36 C37 C38 126.0(6) . . ? N6 C38 C37 116.8(6) . . ? N6 C38 C39 125.6(6) . . ? C37 C38 C39 117.5(6) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C45 120.6(6) . . ? C41 C40 N6 117.7(6) . . ? C45 C40 N6 121.6(6) . . ? C42 C41 C40 118.3(7) . . ? C42 C41 C46 121.0(7) . . ? C40 C41 C46 120.5(6) . . ? C41 C42 C43 122.8(7) . . ? C41 C42 H42 118.6 . . ? C43 C42 H42 118.6 . . ? C44 C43 C42 117.3(7) . . ? C44 C43 C49 121.9(9) . . ? C42 C43 C49 120.8(9) . . ? C43 C44 C45 123.2(7) . . ? C43 C44 H44 118.4 . . ? C45 C44 H44 118.4 . . ? C44 C45 C40 117.9(7) . . ? C44 C45 C52 118.8(7) . . ? C40 C45 C52 123.3(6) . . ? C48 C46 C41 113.4(7) . . ? C48 C46 C47 111.2(7) . . ? C41 C46 C47 110.3(7) . . ? C48 C46 H46 107.2 . . ? C41 C46 H46 107.2 . . ? C47 C46 H46 107.2 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 C51 128.0(9) . . ? C50 C49 C43 120.8(9) . . ? C51 C49 C43 110.7(8) . . ? C50 C49 H49 92.2 . . ? C51 C49 H49 92.2 . . ? C43 C49 H49 92.2 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C45 C52 C54 112.0(6) . . ? C45 C52 C53 110.4(6) . . ? C54 C52 C53 110.2(6) . . ? C45 C52 H52 108.0 . . ? C54 C52 H52 108.0 . . ? C53 C52 H52 108.0 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Cl1 C55 Cl2 110.6(5) . . ? Cl1 C55 Cl3B 134.1(8) . . ? Cl2 C55 Cl3B 93.2(6) . . ? Cl1 C55 Cl3A 93.2(6) . . ? Cl2 C55 Cl3A 118.1(5) . . ? Cl3B C55 Cl3A 41.2(4) . . ? Cl1 C55 H55 111.2 . . ? Cl2 C55 H55 111.2 . . ? Cl3B C55 H55 94.3 . . ? Cl3A C55 H55 111.2 . . ? Cl4 C56 Cl5 111.8(7) . . ? Cl4 C56 Cl6 110.4(6) . . ? Cl5 C56 Cl6 109.8(6) . . ? Cl4 C56 H56 108.2 . . ? Cl5 C56 H56 108.2 . . ? Cl6 C56 H56 108.2 . . ? Cl8 C57 Cl9 111.1(5) . . ? Cl8 C57 Cl7 110.9(4) . . ? Cl9 C57 Cl7 111.2(5) . . ? Cl8 C57 H57 107.8 . . ? Cl9 C57 H57 107.8 . . ? Cl7 C57 H57 107.8 . . ? Cl11 C58 Cl12 110.2(4) . . ? Cl11 C58 Cl10 111.0(4) . . ? Cl12 C58 Cl10 109.6(4) . . ? Cl11 C58 H58 108.7 . . ? Cl12 C58 H58 108.7 . . ? Cl10 C58 H58 108.7 . . ? Cl15 C59 Cl13 109.2(6) . . ? Cl15 C59 Cl14 116.1(6) . . ? Cl13 C59 Cl14 107.9(5) . . ? Cl15 C59 H59 107.8 . . ? Cl13 C59 H59 107.8 . . ? Cl14 C59 H59 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N1 C17 0.9(4) . . . . ? O1 Ni1 N1 C17 -177.3(4) . . . . ? O2 Ni1 N1 C17 -91.2(4) . . . . ? N3 Ni1 N1 C17 -6.1(7) . . . . ? Br1 Ni1 N1 C17 93.8(4) . . . . ? N2 Ni1 N1 C1 -179.1(5) . . . . ? O1 Ni1 N1 C1 2.7(5) . . . . ? O2 Ni1 N1 C1 88.8(5) . . . . ? N3 Ni1 N1 C1 173.9(5) . . . . ? Br1 Ni1 N1 C1 -86.2(5) . . . . ? O1 Ni1 N2 C18 10.2(16) . . . . ? O2 Ni1 N2 C18 92.3(5) . . . . ? N1 Ni1 N2 C18 -0.7(4) . . . . ? N3 Ni1 N2 C18 176.3(5) . . . . ? Br1 Ni1 N2 C18 -96.7(4) . . . . ? O1 Ni1 N2 C22 -169.6(12) . . . . ? O2 Ni1 N2 C22 -87.6(5) . . . . ? N1 Ni1 N2 C22 179.5(5) . . . . ? N3 Ni1 N2 C22 -3.6(4) . . . . ? Br1 Ni1 N2 C22 83.5(4) . . . . ? N2 Ni1 N3 C27 -174.6(6) . . . . ? O1 Ni1 N3 C27 3.0(6) . . . . ? O2 Ni1 N3 C27 -80.5(5) . . . . ? N1 Ni1 N3 C27 -167.6(5) . . . . ? Br1 Ni1 N3 C27 90.6(5) . . . . ? N2 Ni1 N3 C23 5.1(4) . . . . ? O1 Ni1 N3 C23 -177.3(4) . . . . ? O2 Ni1 N3 C23 99.2(4) . . . . ? N1 Ni1 N3 C23 12.1(7) . . . . ? Br1 Ni1 N3 C23 -89.7(4) . . . . ? N5 Ni2 N4 C32 -4.9(4) . . . . ? N6 Ni2 N4 C32 5.8(7) . . . . ? Br2 Ni2 N4 C32 165.3(3) . . . . ? Br3 Ni2 N4 C32 -93.1(4) . . . . ? N5 Ni2 N4 C28 -171.7(5) . . . . ? N6 Ni2 N4 C28 -160.9(5) . . . . ? Br2 Ni2 N4 C28 -1.5(5) . . . . ? Br3 Ni2 N4 C28 100.1(5) . . . . ? N6 Ni2 N5 C37 10.1(4) . . . . ? N4 Ni2 N5 C37 -174.4(4) . . . . ? Br2 Ni2 N5 C37 65.4(10) . . . . ? Br3 Ni2 N5 C37 -84.4(4) . . . . ? N6 Ni2 N5 C33 -178.3(5) . . . . ? N4 Ni2 N5 C33 -2.7(4) . . . . ? Br2 Ni2 N5 C33 -123.0(7) . . . . ? Br3 Ni2 N5 C33 87.2(4) . . . . ? N5 Ni2 N6 C38 -7.9(4) . . . . ? N4 Ni2 N6 C38 -18.7(7) . . . . ? Br2 Ni2 N6 C38 -178.9(4) . . . . ? Br3 Ni2 N6 C38 79.3(4) . . . . ? N5 Ni2 N6 C40 174.1(5) . . . . ? N4 Ni2 N6 C40 163.3(5) . . . . ? Br2 Ni2 N6 C40 3.1(5) . . . . ? Br3 Ni2 N6 C40 -98.7(5) . . . . ? C17 N1 C1 C2 -81.6(7) . . . . ? Ni1 N1 C1 C2 98.4(6) . . . . ? C17 N1 C1 C6 93.4(7) . . . . ? Ni1 N1 C1 C6 -86.6(6) . . . . ? C6 C1 C2 C3 -0.8(9) . . . . ? N1 C1 C2 C3 174.0(5) . . . . ? C6 C1 C2 C7 177.8(6) . . . . ? N1 C1 C2 C7 -7.4(9) . . . . ? C1 C2 C3 C4 0.3(9) . . . . ? C7 C2 C3 C4 -178.4(6) . . . . ? C2 C3 C4 C5 0.3(10) . . . . ? C2 C3 C4 C13 -178.2(6) . . . . ? C3 C4 C5 C6 -0.3(10) . . . . ? C13 C4 C5 C6 178.2(6) . . . . ? C4 C5 C6 C1 -0.2(10) . . . . ? C4 C5 C6 C10 -177.6(6) . . . . ? C2 C1 C6 C5 0.8(9) . . . . ? N1 C1 C6 C5 -174.1(5) . . . . ? C2 C1 C6 C10 178.0(6) . . . . ? N1 C1 C6 C10 3.1(9) . . . . ? C1 C2 C7 C9 -114.9(7) . . . . ? C3 C2 C7 C9 63.7(8) . . . . ? C1 C2 C7 C8 121.0(7) . . . . ? C3 C2 C7 C8 -60.4(8) . . . . ? C5 C6 C10 C11 -57.7(8) . . . . ? C1 C6 C10 C11 125.1(7) . . . . ? C5 C6 C10 C12 67.8(8) . . . . ? C1 C6 C10 C12 -109.3(7) . . . . ? C5 C4 C13 C14 128.1(9) . . . . ? C3 C4 C13 C14 -53.5(10) . . . . ? C5 C4 C13 C15 -100.7(8) . . . . ? C3 C4 C13 C15 77.8(9) . . . . ? C1 N1 C17 C18 179.0(5) . . . . ? Ni1 N1 C17 C18 -1.0(7) . . . . ? C1 N1 C17 C16 -1.4(9) . . . . ? Ni1 N1 C17 C16 178.6(5) . . . . ? C22 N2 C18 C19 -0.1(9) . . . . ? Ni1 N2 C18 C19 -179.9(5) . . . . ? C22 N2 C18 C17 -179.8(5) . . . . ? Ni1 N2 C18 C17 0.3(7) . . . . ? N1 C17 C18 N2 0.6(8) . . . . ? C16 C17 C18 N2 -179.1(6) . . . . ? N1 C17 C18 C19 -179.2(6) . . . . ? C16 C17 C18 C19 1.2(10) . . . . ? N2 C18 C19 C20 1.2(10) . . . . ? C17 C18 C19 C20 -179.1(6) . . . . ? C18 C19 C20 C21 -1.0(11) . . . . ? C19 C20 C21 C22 -0.2(11) . . . . ? C18 N2 C22 C21 -1.2(9) . . . . ? Ni1 N2 C22 C21 178.6(5) . . . . ? C18 N2 C22 C23 -178.4(5) . . . . ? Ni1 N2 C22 C23 1.5(7) . . . . ? C20 C21 C22 N2 1.4(10) . . . . ? C20 C21 C22 C23 178.2(6) . . . . ? C27 N3 C23 C24 -4.2(9) . . . . ? Ni1 N3 C23 C24 176.0(5) . . . . ? C27 N3 C23 C22 173.8(5) . . . . ? Ni1 N3 C23 C22 -6.0(6) . . . . ? N2 C22 C23 N3 3.5(8) . . . . ? C21 C22 C23 N3 -173.5(6) . . . . ? N2 C22 C23 C24 -178.5(6) . . . . ? C21 C22 C23 C24 4.5(10) . . . . ? N3 C23 C24 C25 2.3(9) . . . . ? C22 C23 C24 C25 -175.6(6) . . . . ? C23 C24 C25 C26 1.6(9) . . . . ? C24 C25 C26 C27 -3.4(9) . . . . ? C23 N3 C27 C26 2.4(8) . . . . ? Ni1 N3 C27 C26 -177.9(4) . . . . ? C23 N3 C27 C28 178.0(5) . . . . ? Ni1 N3 C27 C28 -2.2(8) . . . . ? C25 C26 C27 N3 1.4(9) . . . . ? C25 C26 C27 C28 -174.4(6) . . . . ? C32 N4 C28 C29 -3.9(8) . . . . ? Ni2 N4 C28 C29 162.1(4) . . . . ? C32 N4 C28 C27 167.7(5) . . . . ? Ni2 N4 C28 C27 -26.3(7) . . . . ? N3 C27 C28 N4 120.3(6) . . . . ? C26 C27 C28 N4 -63.8(7) . . . . ? N3 C27 C28 C29 -67.9(7) . . . . ? C26 C27 C28 C29 108.0(6) . . . . ? N4 C28 C29 C30 2.9(9) . . . . ? C27 C28 C29 C30 -168.5(6) . . . . ? C28 C29 C30 C31 1.3(9) . . . . ? C29 C30 C31 C32 -4.2(10) . . . . ? C28 N4 C32 C31 0.9(8) . . . . ? Ni2 N4 C32 C31 -167.9(5) . . . . ? C28 N4 C32 C33 179.9(5) . . . . ? Ni2 N4 C32 C33 11.1(6) . . . . ? C30 C31 C32 N4 3.2(10) . . . . ? C30 C31 C32 C33 -175.8(6) . . . . ? C37 N5 C33 C34 0.1(9) . . . . ? Ni2 N5 C33 C34 -171.2(4) . . . . ? C37 N5 C33 C32 -179.3(5) . . . . ? Ni2 N5 C33 C32 9.4(7) . . . . ? N4 C32 C33 N5 -13.8(8) . . . . ? C31 C32 C33 N5 165.2(5) . . . . ? N4 C32 C33 C34 166.8(6) . . . . ? C31 C32 C33 C34 -14.2(9) . . . . ? N5 C33 C34 C35 0.2(9) . . . . ? C32 C33 C34 C35 179.6(6) . . . . ? C33 C34 C35 C36 0.0(10) . . . . ? C34 C35 C36 C37 -0.6(10) . . . . ? C33 N5 C37 C36 -0.7(9) . . . . ? Ni2 N5 C37 C36 170.7(4) . . . . ? C33 N5 C37 C38 178.0(5) . . . . ? Ni2 N5 C37 C38 -10.6(7) . . . . ? C35 C36 C37 N5 0.9(9) . . . . ? C35 C36 C37 C38 -177.6(6) . . . . ? C40 N6 C38 C37 -177.0(5) . . . . ? Ni2 N6 C38 C37 4.8(7) . . . . ? C40 N6 C38 C39 1.1(9) . . . . ? Ni2 N6 C38 C39 -177.1(5) . . . . ? N5 C37 C38 N6 3.2(8) . . . . ? C36 C37 C38 N6 -178.2(6) . . . . ? N5 C37 C38 C39 -175.1(5) . . . . ? C36 C37 C38 C39 3.5(9) . . . . ? C38 N6 C40 C41 101.9(7) . . . . ? Ni2 N6 C40 C41 -80.3(7) . . . . ? C38 N6 C40 C45 -81.4(8) . . . . ? Ni2 N6 C40 C45 96.5(7) . . . . ? C45 C40 C41 C42 1.5(10) . . . . ? N6 C40 C41 C42 178.3(6) . . . . ? C45 C40 C41 C46 177.7(6) . . . . ? N6 C40 C41 C46 -5.5(9) . . . . ? C40 C41 C42 C43 -0.7(11) . . . . ? C46 C41 C42 C43 -176.9(7) . . . . ? C41 C42 C43 C44 -0.2(12) . . . . ? C41 C42 C43 C49 179.1(7) . . . . ? C42 C43 C44 C45 0.3(12) . . . . ? C49 C43 C44 C45 -178.9(7) . . . . ? C43 C44 C45 C40 0.4(11) . . . . ? C43 C44 C45 C52 178.6(7) . . . . ? C41 C40 C45 C44 -1.3(9) . . . . ? N6 C40 C45 C44 -178.0(6) . . . . ? C41 C40 C45 C52 -179.4(6) . . . . ? N6 C40 C45 C52 3.9(10) . . . . ? C42 C41 C46 C48 -46.6(10) . . . . ? C40 C41 C46 C48 137.3(7) . . . . ? C42 C41 C46 C47 78.8(9) . . . . ? C40 C41 C46 C47 -97.3(8) . . . . ? C44 C43 C49 C50 -108.8(15) . . . . ? C42 C43 C49 C50 72.0(16) . . . . ? C44 C43 C49 C51 78.4(11) . . . . ? C42 C43 C49 C51 -100.8(11) . . . . ? C44 C45 C52 C54 -56.2(9) . . . . ? C40 C45 C52 C54 121.9(7) . . . . ? C44 C45 C52 C53 67.1(8) . . . . ? C40 C45 C52 C53 -114.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.996 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.109